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DoD Environmental Field

Sampling Handbook
Revision 1.0

April 2013

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DoD Environmental Field Sampling Handbook


Revision 1

Preface
This handbook provides basic guidance for working-level environmental field sampling personnel to
ensure the integrity of monitoring activities tied to regulatory reporting requirements. The handbook
was developed as a tool for Department of Defense (DoD) personnel. In cases where a contractor
provides environmental sampling and field testing services, the contractor is responsible for ensuring
self-compliance with all environmental and occupational safety and health laws and regulations. In
certain instances, special requirements may dictate a more rigorous detail, depending on federal, state,
and local regulations. Local field sampling procedures should be compatible with the contents of this
handbook. However, there is no intent for guidance herein to replace standard operating procedures,
which may exist at the local level.
Issues regarding the contents of this handbook should be brought to the attention of the DoD Environmental Data Quality Workgroup, Field Sampling and Testing Subgroup.
The DoD Environmental Data Quality Workgroup (EDQW) developed this handbook to provide guidance for environmental field sampling personnel and laboratories performing services for the DoD. It is
based on the Navy Environmental Compliance Sampling and Field Testing Procedures Manual (August
2009), and is expanded to incorporate DoD-wide field sampling and testing guidance. Nothing in this
document relieves any field or laboratory personnel from complying with more stringent contract specifications, host-nation final governing standards, or federal, state, and local regulations. This handbook
can and should be supplemented by project-specific requirements. The DoD EDQW strongly encourages project teams to involve laboratories, project chemists, and field personnel during projectplanning activities. The involvement of the laboratories, field personnel, and project chemists is critical
to the development of project-specific measurement performance criteria (MPC) and to the selection of
methods capable of satisfying the MPC.

Preface

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TABLE OF CONTENTS
Preface ....................................................................................................................................................................... i
Chapter 1. Introduction ......................................................................................................................................... 1-1
1.1. Purpose ................................................................................................................................................. 1-1
1.2. Scope .................................................................................................................................................... 1-1
1.3. Background .......................................................................................................................................... 1-1
1.4. Requirements for Laboratory Testing.................................................................................................. 1-1
1.4.1. Compliance Testing ......................................................................................................................... 1-2
1.4.2. Restoration Testing .......................................................................................................................... 1-2
1.5. Handbook Overview ............................................................................................................................ 1-2
Chapter 2. Sampling and Field Testing Program Overview................................................................................ 2-1
2.1. Purpose ................................................................................................................................................. 2-1
2.2. Need for Proper Planning..................................................................................................................... 2-1
2.3. Systematic Planning and the Conceptual Site Model (CSM) ............................................................. 2-1
2.4. Aerial Photo and Map Analysis ........................................................................................................... 2-2
2.5. Fate and Transport................................................................................................................................ 2-3
2.6. Geophysical Exploration ...................................................................................................................... 2-3
2.7. Data Quality Objectives (DQO) Process ............................................................................................. 2-3
2.7.1. Sampling Strategy ............................................................................................................................ 2-4
2.7.2. Selecting a Sampling Design ........................................................................................................... 2-5
2.7.3. Background Samples ....................................................................................................................... 2-7
2.7.4. Collecting Effective Data ................................................................................................................ 2-9
2.8. Selecting the Project Team .................................................................................................................. 2-9
2.9. Developing a SAP .............................................................................................................................. 2-10
2.10. Health and Safety Plan....................................................................................................................... 2-11
2.10.1. Service-Specific Safety and Occupational (SOH) Health Program ........................................... 2-11
Chapter 3. Common Sampling Procedures .......................................................................................................... 3-1
3.1. Purpose ................................................................................................................................................. 3-1
3.2. Preparations for Field Sampling .......................................................................................................... 3-1
3.2.1. Preparing for a Sampling Event ...................................................................................................... 3-2
3.2.2. Preliminary On-Site Evaluation ...................................................................................................... 3-3
3.2.3. Preliminary Site Safety Evaluation ................................................................................................. 3-3
3.2.4. Explosive Safety Evaluation............................................................................................................ 3-4
3.2.5. Preliminary Sampling Evaluation ................................................................................................... 3-4
3.3. The Sampling Event ............................................................................................................................. 3-4
3.4. Sampling Procedures............................................................................................................................ 3-4
3.4.1. Sampling Strategies ......................................................................................................................... 3-5
3.4.2. Sampling Procedure Checklist ........................................................................................................ 3-5
3.5. Sample Documentation and COC Procedures..................................................................................... 3-6
3.5.1. Pre-Assigned Sample Numbers ....................................................................................................... 3-6
3.5.2. Sample Container Labeling ............................................................................................................. 3-7
3.5.3. FLB/FN ............................................................................................................................................ 3-7
3.5.4. Field Notes/Field Sampling Forms ................................................................................................. 3-9
3.5.5. Chain of Custody (COC) ............................................................................................................... 3-10
3.5.6. Request for Analysis ...................................................................................................................... 3-16
3.6. Sample Packaging, Handling, and Transportation ............................................................................ 3-16
3.6.1. Sample Packaging Requirements .................................................................................................. 3-17
3.6.2. Marking and Labeling.................................................................................................................... 3-23
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3.6.3. Shipping Papers ............................................................................................................................. 3-23


3.7. QA/QC Protocol ................................................................................................................................. 3-23
3.7.1. Decontamination of Sampling Equipment .................................................................................... 3-24
3.7.2. Sample Container Cleanliness Requirements ............................................................................... 3-24
3.7.3. Sample Container Type and Size Requirements........................................................................... 3-24
3.7.4. Sample Preservation and Storage Requirements .......................................................................... 3-25
3.7.5. Sample Holding Time Limits ........................................................................................................ 3-25
3.7.6. Laboratory and Field Analytical Procedures ................................................................................ 3-25
3.7.7. QC Samples ................................................................................................................................... 3-25
3.7.8. Field Audits .................................................................................................................................... 3-27
3.8. Generic Sampling Equipment List..................................................................................................... 3-28
Chapter 4. Soil Sampling ...................................................................................................................................... 4-1
4.1. Purpose ................................................................................................................................................. 4-1
4.2. Scope .................................................................................................................................................... 4-1
4.3. Project Planning ................................................................................................................................... 4-1
4.3.1. Sampling Strategy ............................................................................................................................ 4-1
4.3.2. Site-Specific SAP ............................................................................................................................ 4-3
4.3.3. QA .................................................................................................................................................... 4-4
4.4. Hazards and Safety Precautions ........................................................................................................... 4-5
4.4.1. General Safety.................................................................................................................................. 4-5
4.4.2. Subsurface Hazards ......................................................................................................................... 4-6
4.4.3. Explosive Hazards ........................................................................................................................... 4-7
4.5. Principles of Sample Collection........................................................................................................... 4-7
4.5.1. Preparation of Site Map ................................................................................................................... 4-9
4.5.2. Preliminary Tests and Observations .............................................................................................. 4-10
4.6. Methods of Accessing Soils ............................................................................................................... 4-14
4.6.1. Surface Samples ............................................................................................................................. 4-14
4.6.2. Subsurface Samples ....................................................................................................................... 4-14
4.6.3. Subsurface Geological/Geotechnical Characterization ................................................................ 4-18
4.6.4. Use of Soil Sampling Equipment .................................................................................................. 4-19
4.7. Soil Sampling Procedures .................................................................................................................. 4-23
4.7.1. Preparation ..................................................................................................................................... 4-23
4.7.2. Sample Collection .......................................................................................................................... 4-24
4.7.3. Composite Sampling...................................................................................................................... 4-26
4.7.4. Sample Handling and Preparation ................................................................................................. 4-27
4.8. Restoration of Sample Locations ....................................................................................................... 4-29
4.8.1. Backfill Sample Holes ................................................................................................................... 4-29
4.8.2. Grouting Boreholes ........................................................................................................................ 4-29
4.8.3. Replace Sod ................................................................................................................................... 4-29
4.8.4. Replace Pavement .......................................................................................................................... 4-29
4.9. Decontamination ................................................................................................................................ 4-29
4.9.1. Decontamination Solutions and Supplies...................................................................................... 4-30
4.9.2. Procedure ....................................................................................................................................... 4-30
4.9.3. Preparation of Equipment Rinsate Blanks .................................................................................... 4-33
4.10. Waste Material Storage and Disposal ............................................................................................... 4-33
4.10.1. Soil Cuttings................................................................................................................................. 4-33
4.10.2. Used Disposable PPE .................................................................................................................. 4-33
4.11. Sampling Equipment List .................................................................................................................. 4-33
4.12. References .......................................................................................................................................... 4-34
Chapter 5. Aquatic Sediment Sampling ............................................................................................................... 5-1
5.1.

Purpose ................................................................................................................................................. 5-1

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5.2. Scope .................................................................................................................................................... 5-1


5.3. Project Planning for Sediment-Related Sampling ............................................................................... 5-1
5.3.1. Identify Project Goals ...................................................................................................................... 5-1
5.3.2. Determine Data Needs ..................................................................................................................... 5-2
5.3.3. Develop Data Collection Options.................................................................................................... 5-3
5.4. Developing a Sampling Strategy ......................................................................................................... 5-6
5.5. Methods for Bulk Sediment Sampling ................................................................................................ 5-7
5.5.1. Sediment Grab Sampling Methods ................................................................................................. 5-7
5.5.2. Sediment Core Sampling Methods.................................................................................................. 5-8
5.6. Bulk Sediment Handling and Analysis .............................................................................................. 5-10
5.7. Methods for Collection of Pore Water............................................................................................... 5-11
5.8. Benthic Macroinvertebrate Investigations ......................................................................................... 5-16
5.8.1. Benthic Habitat Mapping............................................................................................................... 5-23
5.8.2. Toxicity Testing in Microcosms or Mesocosms ........................................................................... 5-23
5.9. References .......................................................................................................................................... 5-26
Chapter 6. Surface Water Sampling ..................................................................................................................... 6-1
6.1. Purpose ................................................................................................................................................. 6-1
6.2. Scope .................................................................................................................................................... 6-1
6.3. Project Planning ................................................................................................................................... 6-1
6.3.1. Sampling Strategy ............................................................................................................................ 6-1
6.3.2. Site-Specific SAP ............................................................................................................................ 6-1
6.3.3. QA .................................................................................................................................................... 6-2
6.4. Hazards and Safety Precautions ........................................................................................................... 6-2
6.5. Field Preparation .................................................................................................................................. 6-3
6.5.1. Representative Sampling Considerations........................................................................................ 6-3
6.5.2. Point Source Investigations ............................................................................................................. 6-4
6.5.3. Nonpoint Source Investigations ...................................................................................................... 6-4
6.5.4. Leachate ........................................................................................................................................... 6-5
6.5.5. Wetland Sampling ........................................................................................................................... 6-6
6.6. Sampling Procedures............................................................................................................................ 6-6
6.6.1. Operation of Sample Collection Devices ........................................................................................ 6-7
6.6.2. Sample Collection Procedures....................................................................................................... 6-12
6.7. Sampling Equipment List................................................................................................................... 6-13
Chapter 7. Storm Water Sampling ....................................................................................................................... 7-1
7.1. Purpose ................................................................................................................................................. 7-1
7.2. Storm Water Program Overview ......................................................................................................... 7-1
7.2.1. Regulatory Summary ....................................................................................................................... 7-1
7.2.2. Permitting Requirements ................................................................................................................. 7-3
7.3. Storm Water Compliance ..................................................................................................................... 7-4
7.3.1. Development of a SWPPP ............................................................................................................... 7-5
7.3.2. Compliance Monitoring at Industrial Sites ..................................................................................... 7-6
7.4. Visual Monitoring of Storm Water from Industrial Facilities ............................................................ 7-8
7.5. Collection of Storm Water Samples .................................................................................................... 7-8
7.5.1. Sampling Locations ......................................................................................................................... 7-9
7.5.2. Staffing Considerations ................................................................................................................. 7-10
7.5.3. Sample Type: Grab and Composite Storm Water Samples......................................................... 7-12
7.5.4. Storm Water Sampling from Retention Ponds.............................................................................. 7-13
7.6. Obtaining Flow Data .......................................................................................................................... 7-15
7.6.1. Measuring Flow Rates ................................................................................................................... 7-15
7.7. Compliance Monitoring at Construction Sites .................................................................................. 7-17
7.7.1. Known or Should Be Known Pollutants at Construction Sites ................................................ 7-17
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7.7.2. Deciding When Sampling Is Required at Construction Sites ....................................................... 7-17


7.7.3. When Sampling and Analysis May Not Be Required at Construction Sites ............................... 7-18
7.7.4. When Sampling and Analysis May Be Required at the Construction Site .................................. 7-18
7.7.5. Deciding Where to Sample at a Construction Site........................................................................ 7-19
7.7.6. Collection of Construction Storm Water Samples ........................................................................ 7-22
7.7.7. Coupling Visual Observations with Sampling Results................................................................. 7-22
7.7.8. Retention of Data ........................................................................................................................... 7-23
7.8. Storm Water Sampling Equipment .................................................................................................... 7-23
7.9. Hazards and Safety Pre-Warnings ..................................................................................................... 7-23
7.10. QA/QC ............................................................................................................................................... 7-23
7.11. Sampling Equipment List .................................................................................................................. 7-24
Chapter 8. Groundwater Sampling ....................................................................................................................... 8-1
8.1. Purpose ................................................................................................................................................. 8-1
8.2. Scope .................................................................................................................................................... 8-1
8.3. Project Planning ................................................................................................................................... 8-1
8.3.1. Sampling Strategy ............................................................................................................................ 8-1
8.3.2. Site-Specific SAP ............................................................................................................................ 8-1
8.3.3. QA .................................................................................................................................................... 8-2
8.4. Hazards and Safety Precautions ........................................................................................................... 8-4
8.4.1. General Safety.................................................................................................................................. 8-4
8.4.2. Subsurface Hazards ......................................................................................................................... 8-4
8.5. Field Preparation .................................................................................................................................. 8-5
8.5.1. Access and Identification................................................................................................................. 8-5
8.5.2. Sampling Equipment Selection ....................................................................................................... 8-5
8.5.3. Equipment Cleaning and Decontamination .................................................................................... 8-6
8.6. Sampling Monitoring Wells................................................................................................................. 8-7
8.6.1. Field Measurements ......................................................................................................................... 8-7
8.6.2. Well Development and Purging ...................................................................................................... 8-8
8.6.3. Pumps ............................................................................................................................................. 8-12
8.6.4. Groundwater Sampling Procedures Using Monitoring Wells...................................................... 8-15
8.6.5. Overview of Passive Groundwater Sampling in Monitor Wells .................................................. 8-16
8.7. In Situ Groundwater Sampling Using Probes ................................................................................... 8-20
8.7.1. In situ Well Installation.................................................................................................................. 8-21
8.7.2. Point-in-Time Sampling ................................................................................................................ 8-21
8.7.3. DPT Monitoring Well Installation ................................................................................................ 8-22
8.8. Sample Handling and Collection ....................................................................................................... 8-23
8.8.1. Sampling for Metals ...................................................................................................................... 8-23
8.8.2. Sampling for VOCs ....................................................................................................................... 8-24
8.8.3. Sampling for Extractable Organics ............................................................................................... 8-24
8.8.4. Sampling for Cyanide .................................................................................................................... 8-24
8.8.5. Sampling for Conventional Parameters and Nutrients ................................................................. 8-25
8.8.6. Sampling for Radioactive Elements .............................................................................................. 8-25
8.8.7. Sampling for Light, Non-aqueous Phase Liquids ......................................................................... 8-26
8.8.8. Sampling for Dense, Non-aqueous Phase Liquids (DNAPLs)..................................................... 8-27
8.9. Sampling Industrial Wells.................................................................................................................. 8-27
8.10. Aquifer Testing .................................................................................................................................. 8-27
8.11. Well Decommissioning or Abandonment ......................................................................................... 8-28
8.12. Sampling Equipment List .................................................................................................................. 8-28
Chapter 9. Drinking Water Sampling................................................................................................................... 9-1
9.1.
9.2.

Purpose ................................................................................................................................................. 9-1


Background .......................................................................................................................................... 9-1

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9.3. Scope .................................................................................................................................................... 9-2


9.4. Project Planning ................................................................................................................................... 9-3
9.4.1. Sampling Strategy ............................................................................................................................ 9-3
9.4.2. Site-Specific SAP ............................................................................................................................ 9-3
9.4.3. Certification ..................................................................................................................................... 9-3
9.4.4. Analytical Methods.......................................................................................................................... 9-4
9.4.5. Quality Assurance ............................................................................................................................ 9-4
9.5. Hazards and Safety Precautions ........................................................................................................... 9-4
9.6. General Sampling Procedures .............................................................................................................. 9-5
9.6.1. General Tap Sampling ..................................................................................................................... 9-5
9.6.2. Service Line Sampling..................................................................................................................... 9-6
9.6.3. First-Draw Sampling ....................................................................................................................... 9-7
9.6.4. Source Water Sampling (Surface Water) ...................................................................................... 9-7
9.6.5. Source Water Sampling From a Well ............................................................................................. 9-8
9.7. Parameter-Specific Sampling Procedures ........................................................................................... 9-9
9.7.1. Field Data ......................................................................................................................................... 9-9
9.7.2. Microbiological .............................................................................................................................. 9-10
9.7.3. Metals ............................................................................................................................................. 9-14
9.7.4. Nitrates/Nitrites. ............................................................................................................................. 9-16
9.7.5. Pesticides and Synthetic Organic Chemicals ................................................................................ 9-17
9.7.6. DBPs .............................................................................................................................................. 9-18
9.7.7. Radionuclides................................................................................................................................. 9-19
9.8. Sampling Equipment List................................................................................................................... 9-21
Chapter 10. Waste Sampling .............................................................................................................................. 10-1
10.1. Purpose ............................................................................................................................................... 10-1
10.2. Scope .................................................................................................................................................. 10-1
10.2.1. USTs............................................................................................................................................. 10-1
10.2.2. PCBs............................................................................................................................................. 10-2
10.2.3. Containers and Drums ................................................................................................................. 10-2
10.2.4. Oil Spills ...................................................................................................................................... 10-3
10.2.5. Solid and Hazardous Waste Characterization ............................................................................. 10-3
10.2.6. Sewage Sludge ............................................................................................................................. 10-5
10.2.7. IDW .............................................................................................................................................. 10-5
10.3. Hazard and Safety Precautions .......................................................................................................... 10-5
10.3.1. Container Hazards ....................................................................................................................... 10-5
10.3.2. USTs and Other Confined Spaces ............................................................................................... 10-5
10.3.3. Explosive Hazards ....................................................................................................................... 10-6
10.4. Preparation ......................................................................................................................................... 10-6
10.4.1. Preparation for UST Sampling .................................................................................................... 10-6
10.4.2. Preparation for PCB Sampling .................................................................................................... 10-6
10.4.3. Preparation for Drum Sampling .................................................................................................. 10-6
10.4.4. Preparation for Cylinder Sampling ............................................................................................. 10-8
10.4.5. Preparation for Storage Tank, Vacuum Truck, Process Vessel, and Similar Large Container
Sampling................................................................................................................................................... 10-8
10.5. Sample Collection Procedures........................................................................................................... 10-9
10.5.1. Large Tanks ................................................................................................................................. 10-9
10.5.2. Secondary Containment Sampling .............................................................................................. 10-9
10.5.3. Surficial Sampling ....................................................................................................................... 10-9
10.5.4. Transformers .............................................................................................................................. 10-12
10.5.5. Containerized Liquids................................................................................................................ 10-12
10.5.6. Waste Pile Sampling .................................................................................................................. 10-16
10.5.7. Containerized Solids .................................................................................................................. 10-18
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10.5.8. Sampling for Lead in Paint ........................................................................................................ 10-19


10.5.9. Ashore Oil Spill Sampling......................................................................................................... 10-20
10.6. QA/QC ............................................................................................................................................. 10-21
10.7. Sampling Equipment List ................................................................................................................ 10-21
Chapter 11. Air Sampling ................................................................................................................................... 11-1
11.1. Purpose ............................................................................................................................................... 11-1
11.2. Scope .................................................................................................................................................. 11-1
11.3. Background ........................................................................................................................................ 11-1
11.3.1. Air Matrices ................................................................................................................................. 11-1
11.3.2. Objectives of Air Sampling and Monitoring............................................................................... 11-1
11.4. General Classification of Air Pollutants............................................................................................ 11-2
11.5. Factors Affecting Ambient Air Sampling and Monitoring .............................................................. 11-4
11.5.1. Meteorological ............................................................................................................................. 11-4
11.5.2. Topographical Factors ................................................................................................................. 11-5
11.5.3. Extraneous Contaminant Sources................................................................................................ 11-5
11.5.4. Response Time of Sensors........................................................................................................... 11-5
11.5.5. Placement of Samplers and Monitors ......................................................................................... 11-5
11.6. General Terms.................................................................................................................................... 11-6
11.6.1. Whole Air versus Component Samplers ..................................................................................... 11-6
11.6.2. Real Time versus Integrated or Composite Samplers................................................................. 11-6
11.6.3. Active Versus Passive Samplers ................................................................................................. 11-6
11.7. Strategies for Assessment of Air Pollution Emissions ..................................................................... 11-6
11.7.1. Direct Assessment ....................................................................................................................... 11-6
11.7.2. Indirect Assessment ..................................................................................................................... 11-6
11.7.3. Air Monitoring and Dispersion Modeling .................................................................................. 11-7
11.7.4. Predictive Modeling..................................................................................................................... 11-7
11.8. Field Measurement Instruments ........................................................................................................ 11-7
11.8.1. Detection of Volatile Organic Chemicals (VOCs) ..................................................................... 11-8
11.8.2. Explosimeter .............................................................................................................................. 11-10
11.8.3. Detection of Hydrogen Sulfide (H2S) ....................................................................................... 11-11
11.8.4. Detection of Carbon Monoxide (CO) ....................................................................................... 11-11
11.8.5. Particulates ................................................................................................................................. 11-11
11.8.6. Mercury Vapor........................................................................................................................... 11-11
11.9. Collecting Samples for Laboratory Analysis .................................................................................. 11-11
11.9.1. Whole Air Samples .................................................................................................................... 11-11
11.9.2. Air Component Samples............................................................................................................ 11-13
11.10. Particulates ..................................................................................................................................... 11-17
11.10.1. Filtration ................................................................................................................................... 11-17
11.10.2. Centrifugal Collection and Impaction ..................................................................................... 11-17
11.11. Stationary Source Emission Samples ............................................................................................ 11-18
11.11.1. Special Problems with Stack Vent and Duct Sampling.......................................................... 11-18
11.11.2. Specified Procedures ............................................................................................................... 11-19
11.12. Measurement of Air Volume Sampled ......................................................................................... 11-19
11.12.1. Low Flow Rate Samples.......................................................................................................... 11-20
11.12.2. High Flow Rate Samples ......................................................................................................... 11-20
11.13. Hazard and Safety Precautions ...................................................................................................... 11-20
11.13.1. Environmental Hazards ........................................................................................................... 11-20
11.13.2. Stack, Vent, and Duct Sampling Safety .................................................................................. 11-20
11.13.3. Instrument Hazards .................................................................................................................. 11-20
11.14. Preparation for Sampling ............................................................................................................... 11-21
11.14.1. Role of the Sampler ................................................................................................................. 11-21
11.14.2. Guidelines for Air Sampling ................................................................................................... 11-21
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Chapter 12. Process Sampling ............................................................................................................................ 12-1


12.1. Purpose ............................................................................................................................................... 12-1
12.2. Scope .................................................................................................................................................. 12-1
12.3. Ex situ Groundwater Treatment ........................................................................................................ 12-1
12.3.1. Liquid-Phase Granular Activated Carbon ................................................................................... 12-1
12.3.2. Air Stripping ................................................................................................................................ 12-1
12.4. In situ Groundwater Treatment ......................................................................................................... 12-2
12.4.1. Monitored Natural Attenuation (MNA) ...................................................................................... 12-2
12.4.2. Enhanced Anaerobic Bioremediation (EAB).............................................................................. 12-3
12.4.3. Aerobic Biodegradation via Oxygen-Releasing Chemicals ....................................................... 12-4
12.4.4. Air Sparging ................................................................................................................................. 12-5
12.4.5. In situ Thermal Remediation ....................................................................................................... 12-5
12.5. Ex situ Soil Treatment ....................................................................................................................... 12-5
12.5.1. Off-Site Disposal ......................................................................................................................... 12-5
12.5.2. Landfarming................................................................................................................................. 12-6
12.5.3. Solidification/Stabilization .......................................................................................................... 12-6
12.5.4. Low-Temperature Thermal Desorption ...................................................................................... 12-6
12.6. In situ Soil Treatment ........................................................................................................................ 12-7
12.6.1. Soil Vapor Extraction (SVE) ....................................................................................................... 12-7
12.6.2. Bioventing .................................................................................................................................... 12-7
12.6.3. In situ Thermal Remediation. ...................................................................................................... 12-7
12.7. Chemical and Physical Parameters for Remediation Processes ....................................................... 12-7
12.8. References .......................................................................................................................................... 12-8
Chapter 13. Field Testing ................................................................................................................................... 13-1
13.1.
13.2.
13.3.
13.4.
13.5.
13.6.
13.7.

Purpose ............................................................................................................................................... 13-1


Scope .................................................................................................................................................. 13-1
Background ........................................................................................................................................ 13-1
Training .............................................................................................................................................. 13-1
Field Screening .................................................................................................................................. 13-1
Field Operations ................................................................................................................................. 13-2
Sample SOPs...................................................................................................................................... 13-2

Chapter 14. Guidelines for Requesting Laboratory Testing .............................................................................. 14-1


14.1.
14.2.
14.3.
14.4.
14.5.
14.6.
14.7.
14.8.
14.9.
14.10.

Purpose ............................................................................................................................................... 14-1


Scope .................................................................................................................................................. 14-1
Responsibilities .................................................................................................................................. 14-1
Hazards and Safety Precautions ........................................................................................................ 14-2
Planning.............................................................................................................................................. 14-2
Parameters and Analytical Methods.................................................................................................. 14-3
Laboratory Selection.......................................................................................................................... 14-4
QA/QC ............................................................................................................................................... 14-5
Reporting............................................................................................................................................ 14-5
Project Schedule Considerations ..................................................................................................... 14-7

Appendix A. Sampler/Sampling Recommendations and Strategies ............................................................... A-1


Appendix B. Requirements for Sample Containers, Preservation, and Holding Times................................ B-1
Appendix C. Requirements for Collection of Quality Control Samples........................................................ C-1
Acronyms .................................................................................................................................................................. i
Glossary of Terms..................................................................................................................................................... i
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Chapter 1. Introduction
1.1. Purpose
The purpose of the DoD Environmental Sampling
Handbook is to provide general sampling guidance and promote consistency in how environmental samples are collected and analyzed. The
handbook discusses strategies and techniques that
can be employed to sample and analyze various
media, including but not limited to water, soils,
gas, and tissues. Applications and limitations of
each sampling strategy and technique are briefly
described. This handbook is not intended to be
all inclusive, but it does provide guidance and
discussion of basic sampling techniques. Many
of the techniques discussed in this handbook have
been derived from approved and accepted regulatory programs. When appropriate, references to
standardized methods are provided.
1.2. Scope
This handbook describes techniques that can be
used for environmental sampling and analysis at
Department of Defense (DoD) compliance, restoration, or other sites. Handbook users are cautioned on possible differences between material
presented here and requirements contained in
control documents such as permits, licenses, state,
local, and other countries program regulations.
These control documents have legal precedence
and may prescribe sampling practices unique to a
specific program or site. When sampling to
document compliance with a control document
(regulation, permit, etc.), the control document
takes precedence over this handbook, and this
handbook should be used as a guidance document
only.
1.3. Background
Accurate, defensible, environmental sampling
and field-testing results are imperative for regulatory compliance monitoring. There is great opportunity for error considering the variable conditions within the environment and the great variety
of sampling equipment available. There is little
tolerance for error since the validity of associated
laboratory test results depends on
Chapter 1 Introduction

sample integrity. Sampling personnel are key to


the success of environmental sampling and testing programs upon which decisions are based.
At times, sampling personnel interface directly
with federal, state, and local oversight personnel
while sampling. They play sensitive roles in
representing their commands and activities in this
manner. At all times, success requires that sampling personnel be familiar with governing directives and their roles in relation to them, that they
be properly trained and qualified, and specifically, that they have a strong appreciation for:

The environmental sampling organization

The importance of sampling plans

Sampling and laboratory personnel interface

Sampling equipment usage and maintenance


requirements

Sampling and field testing procedures

Record and log keeping requirements

Chain-of-custody (COC) requirements

Personnel and equipment safety precautions

Labeling, preservation, packaging, and


shipping requirements

Training and qualification requirements.

This handbook responds to the above concerns by


providing clear, concise, and consistent guidance
to sampling personnel. It provides the framework
to identify generic requirements pertaining to
sampling, to the extent possible, given the diverse
missions and sites of the DoD, and is designed to
augment and improve internal management of
DoD environmental sampling programs. It is not
intended to create any right or benefit, substantive
or procedural, enforceable at law by any party
against the DoD, its officers, employees, or any
person.
1.4. Requirements for Laboratory Testing
An important element of the DoDs mission is to
prevent environmental pollution, protect human
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health and the environment, and comply with


regulations established by federal, state, local,
and tribal governments. To document the results
of the DoDs efforts in protecting human health
and the environment, and to substantiate compliance with environmental regulations, the DoD
procures environmental laboratory testing services. These services consist of two significant
components:

Assessing regulatory compliance of materials,


systems, and processes
Evaluating effectiveness of environmental
restoration efforts.
1.4.1. Compliance Testing
The DoD has a continual need for laboratory
testing services to evaluate compliance with
regulatory limits defined for environmental pollutants. The DoD requires compliance testing to
conform with the following environmental laws:
RCRA

Resource Conservation and Recovery Act

CWA

Clean Water Act

TSCA

Toxic Substances Control Act

SDWA

Safe Drinking Water Act

FIFRA

Federal Insecticide, Fungicide, and


Rodenticide Act

CAA

Clean Air Act

Note: The Emergency Planning and Community Right-toKnow Act (EPCRA) and Executive Order 12856 may place
some additional demands on the laboratories.
These laws prescribe analyses of potable and non-potable
water systems, hazardous and toxic materials, and air
emissions. To comply with these regulations, the DoD
operates its facilities pursuant to regulatory requirements
that address process discharges. Permits may be required
for base support systems (dry docks, sewer, water, industrial waste treatment) and production processes (painting,
degreasing, abrasive blasting, flushing). The DoD accomplishes environmental analysis through both in-house and
commercial laboratories.

1.4.2. Restoration Testing


Restoration testing is conducted pursuant to
requirements in the following laws:

Chapter 1 Introduction

CERCLA

Comprehensive Environmental
Response, Compensation, and Liability Act

SARA

Superfund Amendments and Reauthorization Act of 1986

RCRA

Resource Conservation and Recovery Act

Restoration testing is performed almost exclusively by commercial laboratories. Restoration


work is accomplished by using prime contractors
that sub-contract analytical work to commercial
laboratories. The laboratories are nominated by
the prime contractor and approved by the DoD.
Laboratories performing testing in support of the
DoD environmental restoration programs must be
accredited in accordance with the DoD Environmental Laboratory Accreditation Program
(ELAP). DoD ELAP ensures laboratories performing analyses for the environmental restoration program meet a minimum quality standard.
A project-specific audit of the laboratory's ability
to meet project-specific requirements may also be
performed. Additionally, unannounced data
package audits may be completed to ensure quality data is being submitted after the laboratory has
been approved.
1.5. Handbook Overview
Chapter 1 Summarizes the handbook and gives
direction for its use.
Chapter 2 Provides an overview of the sampling program in general. This chapter is intended to provide sampling personnel with guidance concerning a sampling program, responsibilities of all personnel in the sampling program, as
well as the documentation required by the United
States (U.S.) Environmental Protection Agency
(EPA) for each sampling event.
To sampling personnel, Chapters 3 through 12
represent the core of the handbook by providing the procedures and requirements of field
sampling. A single sampling run will involve the
following sections; see Figure 1-1:
Chapter 3 Common Sampling Procedures

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Chapter 4 12 Soil, Sediment, Surface Water,


Storm Water, Groundwater, Drinking Water,
Waste, and Process Sampling
Chapter 13 Field Testing
Chapter 14 Guidelines for Requesting
Laboratory Testing
Appendix A Sampler/Sampling
Recommendations and Strategies
Appendix B Requirements for Sample
Containers, Preservation, and Holding Times
Appendix C Requirements for Collection of
Quality Control Samples

Chapter 1 Introduction

Of major importance with any material, is the


ability to quickly locate certain information such
as chapters, key words, subjects, figures, tables,
etc. This handbook accomplishes this task with
the following guides:
Table of Contents provides page numbers for all
major sections and subsections.
List of Figures and List of Tables provide page
numbers for all figures and tables.
Glossary of Terms and Acronyms define
technical words and abbreviations.
Reference Sections provide sources of
information used throughout the handook,
including additional sources of information.

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Figure 1-1. Chapter / Appendix Relationships


Chapter 7
Storm Water
Appendix B
Requirements for
Sample Containers,
Preservation, and
Holding Times

Chapter 8
Groundwater Sampling
Appendix B
Requirements for
Sample Containers,
Preservation, and
Holding Times

Chapter 6
Surface Water
Sampling
Appendix B
Requirements for
Sample Containers,
Preservation, and
Holding Times

Chapter 5
Aquatic Sediment
Sampling
Appendix B
Requirements for
Sample Containers,
Preservation, and
Holding Times

Chapter 10
Waste
Sampling
Appendix B
Requirements for
Sample Containers,
Preservation, and
Holding Times

Chapter 3
Common Sampling
Procedures

Chapter 1 Introduction

Chapter 11
Air Sampling

Chapter 12
Process Sampling
Appendix B
Requirements for
Sample Containers,
Preservation, and
Holding Times

Chapter 4
Soil Sampling
Appendix B
Requirements for
Sample Containers,
Preservation, and
Holding Times

Appendix A
Sampler/Sampling
Recommendations and
Strategies

Chapter 9
Drinking Water
Sampling
Appendix B
Requirements for
Sample Containers,
Preservation, and
Holding Times

Chapter 14
Guidelines
for
Requesting
Laboratory Testing

Appendix B
Requirements for Sample
Containers, Preservation,
and Holding Times

Appendix C
Requirements for Collections
of Quality Control Samples

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THIS PAGE INTENTIONALLY LEFT BLANK

Chapter 1 Introduction

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Chapter 2. Sampling and Field Testing Program Overview


2.1. Purpose
This chapter presents the fundamental components of planning a sampling and analysis program and discusses methods for selecting a sampling design and strategy for collecting environmental data. In addition, guidance is provided on
developing a Sampling and Analysis Plan (SAP).
A well-developed SAP plays a critical role in
ensuring the collection of data that have sufficient
quality from which to make defensible decisions.
Planning is a necessary component of any environmental data collection program. The SAP
should clearly state the purpose of the project,
identify the type, quality, and quantity of data
needed to accomplish project goals, and openly
acknowledge any underlying assumptions or
sources of uncertainty that could significantly
impact the quality of the data.
2.2. Need for Proper Planning
Environmental sampling projects require careful
planning and consideration by the project team to
ensure that resources are effectively used to
collect acceptable data for accomplishing project
goals. The level of detail and amount of time
spent on planning should reflect the importance
and intended use of the data and the resources
available to the project (sometimes referred to as
the graded approach). In any environmental
program, the three following questions need to be
answered before a project is started:

What are the objectives of the project?


How will the data generated ultimately be
used?
What type, quality, and quantity of data are
needed to accomplish the objectives of the
project?
The answers to these questions provide the foundation for determining the proper sampling methodology for the project.

Chapter 2 Sampling and Field Testing Program Overview

2.3. Systematic Planning and the Conceptual


Site Model (CSM)
The Systematic Planning Process is a methodical
approach recommended by the U.S. EPA to:

Identify the technical goals of a project and


site conditions
State the expected outcome of data collection
Outline the cost and schedule of the project
State the acceptance criteria for the final
result.
The essence of systematic planning is accurately
stating the objectives related to an environmental
issue and then strategizing how best to address
those objectives. Successful systematic planning
identifies the key decision makers and allows all
participants in the environmental project to be
aware of the reasoning behind their decisions.
Communication between organizations and individuals involved in an environmental project is
encouraged early in the planning process. This
will ensure that all participants understand the
needs and expectations of the data collection
effort and the questions the project is trying to
answer. Early communication also provides an
efficient use of program resources by requiring a
thorough discussion among the entire project
team of the type, quality, and quantity of data
required to address project goals prior to the start
of the data collection process.
A key tool used in the systematic planning
process is a CSM. A CSM can be defined as a
written and/or pictorial representation of an environmental system and the biological, physical and
chemical processes that determine the fate and
transport of contaminants through environmental
media to environmental receptors and their most
likely exposure models. A CSM promotes
project transparency among the project team by
summarizing all the available information about a
site and identifying what additional information
must be known to achieve project objectives. The
format of a projects CSM may vary.
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A good CSM addresses the following elements as


applicable to the objectives of the project:

Nature and extent of contamination


Geology
Hydrogeology
Fate and transport
Biological and geochemical conditions
Potential transport pathways of contamination
and exposure scenarios
Potential monitoring points
Potential receptors
Potential exposure scenarios and pathways
Potential areas of unacceptable risk
Potential target treatment zones
Site history and intended future site use
Other factors relevant to the understanding of
contamination and related risk to human
health and the environment.
During the systematic planning process, project
goals are linked to the individual activities necessary to reach these goals by identifying data gaps
in the CSM. The CSM then serves as the foundation for evaluating all proposed and implemented
project activities.
The CSM is the basis for defining the Remedial
Action Objectives (RAOs). It also should be used
to expose data gaps and aid in development of the
SAP.
The CSM is used onsite to focus fieldwork efforts
on obtaining the information needed to remove
important unknowns from the model and developing an exit strategy. As site work progresses
and data gaps are filled, the CSM is updated to
reflect the new information. This process allows
the CSM to evolve as the project progresses. The
CSM ultimately serves as a planning tool as well
as a modeling and data interpretation tool. It also
provides a line of communication between field
personnel and the rest of the project team, which
keeps all parties focused on the data collection
process and achieving project objectives.

Chapter 2 Sampling and Field Testing Program Overview

Additional information on CSMs can be found in


the USACE EM 200-1-12, Conceptual Site Models
(http://publications.usace.army.mil/publications/engmanuals/EM_200-1-12/EM_200-1-12.pdf), and the
American Society for Testing and Materials
E1689-95 (2008): Standard Guide for Developing
Conceptual Site Models for Contaminated Sites
(ASTM, 2008).
2.4. Aerial Photo and Map Analysis
As part of the project planning process, current
and historical aerial photos, satellite imagery, and
present-day maps can provide valuable insight
into past and present suspected source areas.
Historical photos may be used to identify past
disposal pits, ground disturbance indicative of
landfills, or stained soil locations that may indicate past spills. Current aerial photos or satellite
imagery may be used to identify potential seeps
for sampling by locating vegetation concentrations in an otherwise dry area. Similarly, the
presence of stressed vegetation may indicate
potential groundwater contamination. In coastline areas, comparing past and present aerial
photos can identify areas of significant shoreline
erosion or aggradation. Source areas that were
located hundreds of feet inland in the 1940s may
now be coastline features. Current aerial photos
and satellite imagery can also be used to infer soil
type and relative permeability of soils present at
the ground surface. Coarse drainage patterns or
broad, shallow valleys may indicate higher permeability soils. Conversely, streams with steep
slopes indicate low permeability soils. Current
aerial photos and satellite imagery can provide
information on the degree of development and
industrialization in the vicinity of source areas,
and can be used to determine potential receptors
and identify potential sample locations.
Guidance for aerial photo analysis may be found
in Aerial Photographs in Geologic Interpretation
and Mapping, U.S. Geological Survey Professional Paper 373.
U.S. EPAs EnviroMapper for Envirofacts website (http://www.epa.gov/emefdata/em4ef.home)
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maps potential waste generators in the project


vicinity and provides information on the types of
waste being generated.
Free imagery can be found at a number of
sources. The Environmental Systems Research
Institute (ESRI) offers two online imagery maps
(World Imagery and Bing Maps Aerial) for inclusion into ArcGIS mapping projects at
http://www.esri.com/data/free-data/index.html
Military installations usually have imagery available also. Army Installation imagery can often be
accessed through the geographic information
system (GIS) or the Department of Public Works
shops. This imagery can be georeferenced and
provide the basis for site sample maps.
2.5. Fate and Transport
Understanding contaminant fate and transport is
an important element of the CSM. In many cases,
the sampling effort or remedial action to address
contamination in soil is based on the potential to
impact groundwater quality or surface water
quality due to the leaching potential. The transport of contaminants via leaching and migration
through groundwater can be a very complex
process. In order to develop a quantitative predictive tool (e.g., a model), geological, geochemical, and hydrogeological data must be available,
including an understanding of seasonal and historical fluctuations in hydrogeological conditions.
Similarly, an understanding of the fate and transport behavior of site contaminants and related
degradation products, particularly in groundwater, is critical to understanding the potential for
contaminant migration and attenuation. This
information is useful in understanding the nature
and extent of any remediation or treatment
processes that may be required to supplement
natural attenuation. These data are used for a risk
assessment and developing risk-based remedial
action objectives for restoration projects and
useful in determining impact for compliance
efforts.

Chapter 2 Sampling and Field Testing Program Overview

2.6. Geophysical Exploration


The use of surface geophysics can be valuable in
planning a sampling program particularly for
choosing sampling locations at suspected source
areas. Geophysical techniques include magnetic
and electromagnetic surveys, ground-penetrating
radar, and seismic surveys. These methods can
help identify buried objects that may represent
sources or sampling hazards, can help define
limits of past excavations or landfills, and can
clarify subsurface hydrogeology that can affect
contaminant transport.
Guidance for the application of geophysics for
contaminated sites is available in United States
Army Corps of Engineers (USACE) Engineer
Manual 1110-1-1802, Geophysical Exploration
for Engineering and Environmental
Investigations
(http://synectics.net/public/file/searchresults.aspx
?dsn=pub&category=USACE&subcategory=Engi
neer%20Manuals&title=USACE%20Engineer%2
0Manuals&idMenu=37839&ddlDSN=SYSTM)
and U.S. EPA documents such as Geophysical
Techniques for Sensing Buried Wastes and Waste
Migration EPA-600/7-84/064 and Subsurface
Characterization and Monitoring Techniques, A
Desk Reference Guide, Volume 1, Chapter 1,
Remote Sensing and Geophysical Methods
EPA/625/R-93/003a, and ASTM Standard
D6429 Standard Guide for Selecting Surface
Geophysical Methods.
2.7. Data Quality Objectives (DQO) Process
The DQO process is a systematic planning tool
recommended by the U.S. EPA to develop sampling designs for data collection activities that
support decision making. The DQO process is a
method used to structure the project planning
processes in order to manage uncertainty. The
DQO process is best applied when critical environmental decisions need to be made (e.g., final
decision-making or compliance with a standard).
The DQO process integrates the work of a multidisciplinary team for planning action-oriented
environmental data collection activities. It encourages thoughtful consideration of the following:
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what decisions need to be made; what data type,


quality, and quantity are needed to support the
decisions; what portion of the environment
(and/or what time frame) shall be represented by
data; how data will be used to support the decision; and what level of decision certainty (and
therefore data quality) is desired. The DQO
process is iterative and the final outcome is a
design for collecting data (e.g., the number of
samples to collect, their locations, and the procedure for sampling). Additionally, acceptable
limits on the probabilities of making decision
errors can be determined if a statistically based
sampling design is used. The full DQO process is
described in the U.S. EPAs Guidance for the
Data Quality Objectives Process (QA/G-4,
EPA/240/B-06/001,
http://www.epa.gov/quality/qs-docs/g4-final.pdf).
The DQO process is a seven-step planning approach based on the scientific method. It involves the entire planning cycle for an environmental project and encompasses all the activities
necessary for project completion. The seven
steps of the DQO process are:
Step 1: State the Problem. Define the problem
clearly, identify the primary decision maker and
planning team members, and determine the available budget, personnel, and deadlines.
Step 2: Identify the Goal of the Study. Develop
an appropriate decision statement, identify the
principal study question, define alternative actions that could result from resolving the principal
study question, link the principal study question
to possible actions, and organize multiple decisions.
Step 3: Identify Information Inputs. Identify
the type and sources of information needed to
resolve the decision statement, identify information needed to establish the action level, and
confirm that suitable methods exist.
Step 4: Define the Boundaries of the Study.
Specify the characteristics that define the population of interest, define the spatial and temporal
boundaries, define the scale of decision making,

Chapter 2 Sampling and Field Testing Program Overview

and identify any practical constraints on data


collection.
Step 5: Develop the Analytic Approach. Construct the theoretical If...then...else... decision
rule by combining the possible results from the
study, the Action Level, the scale of decision
making (Step 4), and the alternative actions (Step
2).
Step 6: Specify Performance or Acceptance
Criteria. Determine the decision makers tolerable limits on potential decision errors by identifying the decision errors and base-level assumptions. Specify a range of possible parameter
values where the consequences of decision errors
are relatively minor, and assign probability values
for the occurrence of potential decision errors.
Step 7: Develop the Detailed Plan for Obtaining Data. Identify a resource-effective sampling
design for data collection that will then satisfy the
DQOs documented in the previous steps. Meeting or exceeding the DQOs is the goal of the
selected sampling design. The DQO process is
flexible and allows the planning team to incorporate new information into the sampling plan as it
becomes available. The final outcomes of the
DQO process are qualitative and quantitative
statements that:

Clarify the study objective


Define the type, quality, and quantity of
required data
Determine the most appropriate conditions
under which to collect the samples
Specify how the data will be used to address
the project objectives.
For more additional information on the DQO
process, see EPA QA/G-4.
2.7.1. Sampling Strategy
Selecting the correct sampling strategy for the
SAP requires consideration of project resources
and an understanding of the data quality required
for the project. When evaluating which sampling
strategy is most appropriate for a given environmental program, project teams should assess the
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amount of time available to complete the project,


the availability of technical experts for on-site
review, the type of data and quality level required
for decision making, and the amount of information already known about the site. Knowing these
key pieces of information will assist project teams
in determining the most appropriate sampling
strategy for the project.
Sampling strategies may be categorized as static or dynamic. Static sampling strategy
represents a phased approach to environmental
data collection. During static sampling, data are
collected and analyzed and then typically documented in an interim report. After the report is
reviewed, the direction of the next phase in the
project is decided. The phased process generally
continues until the project objectives are resolved.
In contrast, dynamic sampling strategy streamlines field sampling activities by providing the
data needed to make decisions on site without
multiple iterations of project work plans and
interim reports. The term dynamic is used because field activities are designed to incorporate
changes as new information is obtained, thus
accommodating the iterative nature of fieldwork
at many environmental sampling sites. The
Triad Approach incorporates dynamic work
strategies, real-time measurements, and systematic planning. More information on the Triad
Approach can be found at
http://www.triadcentral.org/.
A primary advantage of a dynamic sampling
strategy is that it allows an adaptive sampling
approach by encouraging decision makers and
regulators to take an active role in understanding
site problems and resolving sampling issues
quickly. A thorough planning process that clearly
outlines how decisions will be made in the field is
crucial to effectively executing a dynamic sampling program. Dynamic sampling plans are
living documents that provide a roadmap for
decisions that a field team can follow, and outline
how subsequent site activities will progress as
new information is acquired.

Although the benefits of using a dynamic sampling strategy are substantial, they are not applicable for all situations. Dynamic sampling activities often need more extensive planning up front
than traditional staged or static field activities.
Successful dynamic sampling plans should prepare not only for what is known about a site, but
also for possible conditions that could affect the
completion of the fieldwork. Quick turnaround
analysis is typically needed to facilitate dynamic
field activities. If on-site or rapid off-site analysis
is not economically or technically feasible, a
static sampling strategy may be more appropriate.
Dynamic field activities also need more field
oversight, because the regulator should be involved in evaluating key technical decisions as
they occur. In addition, dynamic sampling routinely requires the presence of one or more experienced technical staff in the field. Experienced
staff plays a key role in the decision-making
process, and their recommendations can greatly
influence the direction field activities take. If an
experienced technical team leader is not available
to oversee the fieldwork, dynamic sampling will
often be an ineffective method for data collection.
In this case, a static sampling strategy, which
allows time for review and careful consideration
by technical experts not available for on-site
activities, may be more appropriate.
For additional information on the dynamic sampling process refer to EPA/540/R-03/002
(http://www.epa.gov/superfund/programs/dfa/do
wnload/guidance/40r03002.pdf).
2.7.2. Selecting a Sampling Design
One of the primary objectives of systematic
planning and the DQO process is to determine the
data quality and quantity needed to address
project objectives. Once the data requirements
are identified, the next step in the process is to
develop a sampling design or methodology that
specifies the number, type, and location (spatial
or temporal) of the samples to be selected for
measurement.
There are two main categories of sampling designs: statistical and non-statistical. Statistical

Chapter 2 Sampling and Field Testing Program Overview

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sampling designs apply sampling theory and


involve random selection of sampling locations.
When a statistical sampling design is used, statistical inferences may be made about the sampled
population from the data obtained from the sampling locations. Non-statistical sampling designs
involve the selection of sampling units based on
expert knowledge or professional judgment. Data
derived from non-statistical sample designs cannot be assigned a quantitative level of confidence
and are limited by the degree of professional
knowledge available to the project team.

2.7.2.1. Statistical Sampling Designs


The most commonly used statistical sampling
designs in environmental data collection are:

Simple random sampling. Sample locations


are selected randomly. Locations are
assumed to be independent and have an equal
probability of being selected. Simple random
sampling is most useful when the population
of interest is known or assumed to be
homogeneous. A main advantage of the
simple random sampling design is that it
provides statistically unbiased estimates of the
mean, proportions, and variability.
Stratified random sampling. The target
population is separated into non-overlapping
strata, or subpopulations that are known or
thought to be more homogeneous (relative to
the environmental medium or the
contaminant), so that there tends to be less
variation among the areas sampled in the
same stratum than among sampling areas in
different strata. Strata may be chosen based
on spatial or temporal proximity of the units,
or based on preexisting information or
professional judgment about the site or
process. This design is useful for estimating a
parameter when the target population is
heterogeneous and the area can be subdivided
based on expected contamination levels.
Systematic grid sampling. Samples are
taken at regularly spaced intervals over space
or time. An initial location or time is chosen
at random, and then the remaining sampling

Chapter 2 Sampling and Field Testing Program Overview

locations are defined so that all locations are


at regular intervals over an area (grid) or time
(systematic). This design provides a practical
and easy method for designating sample
locations and ensures uniform coverage of a
site, unit, or process.
Hot-spot sampling or adaptive cluster
sampling. Samples are taken using simple
random sampling, and additional samples are
taken at locations where measurements
exceed some threshold value. Several
additional rounds of sampling and analysis
may be needed. Adaptive sampling is useful
for estimating or searching for rare
characteristics in a population and is
appropriate for inexpensive, rapid
measurements. It enables delineating the
boundaries of hot spots, while also using all
data collected with appropriate weighting to
give unbiased estimates of the population
mean.
Ranked set sampling. Multiple sets of field
locations are identified using simple random
sampling. The locations are ranked
independently within each set using
professional judgment, or an inexpensive, fast
surrogate measurement that is correlated to
the final measurement of interest. One
sampling unit from each set is then selected
(based on the observed ranks) for subsequent
measurement using a more accurate and
reliable method for the contaminant of
interest. Relative to simple random sampling,
this design results in more representative
samples and so leads to more precise
estimates of the population parameters.
Ranked set sampling is useful when the cost
of locating and ranking locations in the field
is low compared to laboratory measurements.
To use a ranked set sampling design
effectively, the ranking method and analytical
method should be strongly correlated.
Incremental Sampling Methodology (ISM).
ISM is based on particulate sampling theory.
It incorporates the relationship that exists
among variability of the soil, particle sizes in
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the soil, the distribution of the contaminant,


and the size of the sample taken.
An incremental sample is similar to but
different from a composite sample. A
composite sample is a combination of discrete
samples. An incremental sample is a
representative sample for a given area to be
sampled (i.e., a decision unit (DU)). An
incremental sample is collected within a DU,
whereas a composite may be collected
without regard to a specific DU. Although
the physical process of collection is similar,
the information derived from each process is
different.
A DU identifies the spatial and temporal
characteristics that define the decisions
domain. Populations are broken into one or
more discrete DUs. The identification and
delineation of the DU is one of the most
important factors when using ISM.
Several benefits of using ISM include
improving the confidence in the mean
concentration in the DU, enabling fewer
samples for shipping and laboratory analysis
(which would result in cost savings), and
providing improved site coverage.
When using ISM, establishing a DU is
critical. In addition, this method can be
difficult to use for volatile contaminants, and
improper selection of a DU may dilute
contamination that could result in
underestimating the need for cleanup. To
ensure achieving the proper results,
consulting a statistician prior to using ISM is
recommended.
For more information regarding ISM, see
Incremental Sampling Methodology,
Interstate Technology & Regulatory Council
(ITRC), 2011.
2.7.2.2. Non-Statistical Sampling Designs
Non-statistical sampling designs are based on
professional judgment, and are usually selected
with the intent of obtaining biased data. For
example, selecting specific locations where a
known spill occurred will provide estimates of the
Chapter 2 Sampling and Field Testing Program Overview

worst case or those of the highest concentrations. Sampling locations are selected based on
visual signs of contamination or previous knowledge about the site. Using a biased sampling
design is most appropriate when dealing with a
known contamination source. The disadvantage
of biased sampling is that contaminated areas
may be overlooked due to inadequate knowledge
of the site or a lack of visual signs of contamination.
For additional information on sampling designs
for environmental data collection, see
EPA/240/R-02/005 QA/G-5S:
http://www.epa.gov/quality1/qs-docs/g5sfinal.pdf).
Visual Sample Plan (VSP) is a software tool that
can be used to employ several of the sampling
strategies previously discussed. VSP supports the
implementation of the DQO process by displaying different sampling plans, linking them to the
DQO process, and then determining the optimal
sampling specifications to protect against potential decision errors.
This easy-to-use program is highly visual, very
graphic, and intended for use by non-statisticians.
The VSP software program may be downloaded
from http://vsp.pnnl.gov/.
2.7.3. Background Samples
In accordance with U.S. EPA guidance, background (reference area) sampling is conducted to
distinguish site-related contamination from naturally occurring or other non-site-related anthropogenic chemicals (EPA, 1989). Background
chemicals can be either localized or widespread
and should be evaluated during site investigations
in order to differentiate between Defense Environmental Restoration Program cleanup responsibilities for site-related releases and background
conditions and/or non-site-related anthropogenic
sources. Both naturally occurring and non-siterelated anthropogenic background levels of chemicals should be established and considered as
early as the Preliminary Assessment/Site Inspection (PA/SI) phase of the CERCLA process or the
Resource Conservation and Recovery Act
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(RCRA) Facility Assessment (RFA) of the RCRA


process.
Establishing scientifically defensible background
levels early in the process can provide evidence
of whether a release has occurred. This technical
position requires a scientifically defensible characterization of background levels of chemicals in
all relevant media that are potentially present at
the site due to background conditions (naturally
occurring and/or non-site-related anthropogenic).
The approach is consistent with the U.S. EPAs
Role of Background in the CERCLA Cleanup
Program (EPA, 2002a), the EPAs Guidance for
Comparing Background and Chemical Concentrations in Soil for CERCLA Sites (EPA, 2002b),
and the U.S. Navys Policy on the Use of Background Chemical Levels (Navy, 2004).
Background is represented by the ambient concentrations of chemicals that are not site-related
or attributable to site releases or activities. This
includes both naturally occurring, and non-siterelated anthropogenic substances present in the
environment. Ideally, background samples
should be geochemically similar to the impacted
portions of the site being evaluated. Soil characteristics such as soil horizon and type, pH, redox
conditions, cation exchange capacity, density,
total organic carbon (TOC), grain size, and moisture are lines of evidence that can be used as
indicators of similarity. Also, background locations should be selected that represent similar
conditions of ambient, anthropogenic contaminants. Sources of anthropogenic background
chemicals that may not be specifically site related
include agricultural runoff, septic systems, application of pesticides, air pollution, industrial discharges, and urban pollution. Background samples are typically taken at upstream locations or
areas not thought to be impacted by the primary
site being investigated.
These non-impacted background or reference
areas identified for sampling may be off-site or
within the designated site boundaries. In order to
reduce the chance of introducing potential sampling bias, background samples should be taken
Chapter 2 Sampling and Field Testing Program Overview

using the same depth and methodologies as those


used for the site investigation. This includes
using the same sample equipment and procedures.
It is also advisable to use the same sampling
personnel and laboratory to perform the analyses.
It is recommended that project teams ensure that
a sufficient number of study areas and background samples be collected to perform proper
statistical tests for the background evaluation.
(Appropriate sample sizes can be determined
using software programs like VSP or ProUCL).
The sampling strategy for background should be
discussed and documented during the early phases of project planning.
A variety of descriptive statistics may be developed to evaluate the background data set (e.g.,
mean, median, range, etc.). Various statistical
tests to compare the mean and/or upper bound
between the site and reference areas require a
sufficient number of reference samples. Geochemical association analysis can also be a valuable tool for background investigations (Navy,
2010). Elemental association relationships can
augment statistical comparisons. It is advisable
that the project team consult a geochemist, chemist, geologist, and/or statistician very early during
project planning to ensure the appropriate chemicals are evaluated as well as the number and
location of selected background samples. These
should be documented in the sampling and analysis plan, which should also specify the project
DQOs and procedures that will be used to collect
the data.
References:

EPA, 2002a. U.S. Environmental Protection


Agency, Role of Background in the CERCLA
Cleanup Program, Office of Solid Waste and
Emergency Response, Washington, D.C.,
OSWER 9285.6-07P, May. This is also included as Appendix B in EPA, 2002b.
EPA, 2002b. U.S. Environmental Protection
Agency, Guidance for Comparing Background
and Chemical Concentrations in Soil for
CERCLA Sites, Office of Emergency and Remedial Response, Washington, D.C., EPA
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540-R-01-003, OSWER 9285.7-41, September.


Navy, 2001. Navy Facilities Engineering
Command (NAVFAC), Guidance for Environmental Background Analysis, Volume I:
Soil, May 3, 2001.
Navy, 2004. Department of the Navy, Navy
Policy on the Use of Background Chemical
Levels, Washington, D.C., 5090, Ser
N45C/N4U732212, 30 January.
2.7.4. Collecting Effective Data
The primary objective when selecting a sampling
design for an environmental program is to determine which design represents the most efficient
methodology for collecting data that are scientifically valid and legally defensible. Data are acceptable when both sampling and analytical
uncertainties have been managed to the degree
necessary to meet accurately defined project
objectives.
While the ability to document the quality of the
data is significant in determining the value of a
data set, the importance of the relationship between data generation and the intended use of the
data cannot be overstated. For example, in a
hypothetical environmental contamination problem (see Figure 2-1) a site contains two hot spot
locations with significantly higher contamination
concentrations than the surrounding area. The
project objective is to identify where the hot spots
are located. Method A analyzes a few samples
using a highly accurate definitive analytical
method that must be sent off site for processing.
Method B surveys the area by analyzing several
samples using a lower quality analytical screening method that can be performed on site. The
additional data points generated using Method B
represents a more effective data set than the data
generated using Method A despite the fact that
Method B data is determined using a lower quality analytical method. Inexpensive or faster
screening methods that meet project DQOs can be
a cost-effective strategy for achieving project
objectives.

Chapter 2 Sampling and Field Testing Program Overview

Figure 2-1. Data Quality vs. Information


Value

Effective data reinforce a more productive conceptual framework for data generation by encouraging critical thinking about the anticipated role
of data. Focusing on achieving effective data
forces the systematic planning process to answer
the following questions:

What is the intended use of the data?


What are the strengths and limitations of the
proposed methods?
What are the site-specific considerations that
could adversely impact analytical
performance?
What are the site-specific considerations that
will influence representative sampling?
What are the site-specific considerations that
will govern what statistical measure should be
determined?

2.8. Selecting the Project Team


Systematic planning is a multidisciplinary process
that requires the participation of the entire project
team early in the planning stages and at key
review points to ensure project resources are used
efficiently. Team members should include the
primary decision makers on the project as well as
the end users of the data to encourage clear communication of data requirements and limitations
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for achieving project goals. Systematic planning


evolves as new information becomes available.
The involvement of the appropriate project team
members at each stage in the process is necessary
to keep the focus on collecting the most effective
data for accomplishing project objectives. Ultimately the planning process is a collaborative
effort that involves the regulator, program managers, field sampling personnel, laboratory personnel, facility health and safety officers, and any
additional individuals involved in the data collection process. Encouraging active participation of
the entire project team is the key to successful
environmental sampling programs.
2.9. Developing a SAP
A SAP is an integral part of the systematic planning process. In general, a site-specific SAP shall
be completed, reviewed, and approved prior to
any data collection. In many cases, the SAP is
not completed before sampling begins and results
in the production of data that may not be usable
for their intended purpose, thus wasting valuable
project resources. It is imperative that project
teams invest the time to complete the DQO
process and prepare a SAP prior to data collection
to increase the likelihood that effective data
will be generated for the project.
At a minimum, each SAP should include the
following sections:

Introduction. Explains the objectives of the


sampling program at the site
Objective. Presents the project objectives,
including the decision criteria applicable to
each parameter analyzed, and describes how
the work will meet these objectives. Explains
the sampling operation in terms of the number
of personnel, education, training, technical
knowledge, and experience needed to meet
assigned functions
Site Description. Provides a description of
the site, including location, current and
historical uses, potential sources of
contamination, and site maps showing the
existing features
Chapter 2 Sampling and Field Testing Program Overview

Conceptual Site Model. Provides information


on both the geology and hydrology at the site,
information on existing water quality and pollutant information, and any known or potential data
gaps
Sample Collection. Explains the types of
samples to be collected, intended methods for
collection, sample handling procedures
(including bottle types, preservation, filtration,
and chain of custody (COC)), analytical
methods, and analytical laboratories
QA/QC. Includes DQOs, field QA/QC
procedures (including sampling equipment
construction, duplicate samples, field blanks,
trip blanks), and requirements for precision,
accuracy, and completeness
Documentation of Field Activities. Includes
field observations and procedures, sample
labeling, and photographic documentation (if
available)
References. Individuals responsible for
preparing the SAP should conduct a site walk
over to familiarize themselves with the field
conditions and, if necessary, consult with
experienced field personnel to obtain input on
appropriate sampling procedures that may be
unique to the site. In addition, the SAP should
incorporate any local regulatory agency
requirements for surface water sampling and
sampling waste management.
SAPs should be prepared based on the regulatory
requirements, the information required for making decisions, and qualifying factors of the sampling and laboratory operations. SAPs describe
the quality system requirements appropriate to
meet the type, range, and scope of the sampling
and testing being performed. Defense Environmental Restoration Program (DERP) projects
must create a SAP following the UFP-QAPP.
The UFP-QAPP format contains all technical and
quality aspects for the life cycle of the project,
including planning, implementation, and assessment. Although only mandatory for DERP
projects, the UFP-QAPP format can also be used
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tional information and guidance on the UFPQAPP can be found at


http://www.epa.gov/fedfac/documents/qualityass
urance.htm.
2.10. Health and Safety Plan
The Health and Safety Plan (HASP) is a separate
deliverable sometimes included with the SAP. A
site-specific HASP meeting the requirements of
29 CFR 1910.120(a)(1)(ii) or (iii) will be included when the scope of work requires it. A
much less extensive site-specific safety plan will
be included for the usual compliance type sampling that does not fall under 29 CFR 1910.120.
2.10.1. Service-Specific Safety and
Occupational (SOH) Health Program
Navy: OPNAVINST 5100.23G, Navy Safety and
Occupational Program Manual, is the primary
reference document describing the Navy SOH
Program. All elements of this handbook apply to
protecting the health and safety of Navy DoD
environmental compliance personnel. The relationship between OSHA standards and the Navy

Chapter 2 Sampling and Field Testing Program Overview

SOH Program is detailed in Chapter 16 of


OPNAVINST 5100.23G.
Army: Army Regulation (AR) 385-10, The Army
Safety Program, implements requirements of the OSH
Act of 1970 as implemented in EO 12196, 29 CFR
1960, DODI 6055.1, DODI 6055.4, and DODI
6055.7. It provides the policy on Army safety management procedures with special emphasis on responsibilities and organizational concepts. This AR applies to the Active Army, the Army National
Guard/Army National Guard of the U.S., and the U.S.
Army Reserve, unless otherwise stated. It also applies
to Army civilian employees and the U.S. Army Corps
of Engineers and Civil Works activities and tenants
and volunteers in accordance with Section 1588, Title
10, U.S. Code and AR 608-1.

Army Corps of Engineers: EM 385-1-1, Safety


and Health Requirements Manual, prescribes the
safety and health requirements for all Corps of
Engineers activities and operations and applies to
occupational exposure for missions under the
command of the Chief of Engineers, whether
accomplished by military, civilian, or contractor
personnel.

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Chapter 2 Sampling and Field Testing Program Overview

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Chapter 3. Common Sampling Procedures


3.1. Purpose
This chapter presents specific sampling procedures and items common to the sampling events
covered in Chapters 4 12. Section 1.5 and
Figure 1-1 of this handbook illustrate the relationships among these chapters. Additional references include facility standard operating procedures (SOPs) and special requirements contained
in regulatory programs and site permits.
3.2. Preparations for Field Sampling
The success of a field sampling program depends
on the level of preparation prior to entering the
field. Implementation of the SAP begins with
preparing for the field sampling operation. The
following preliminary steps are vital to the success of the project:

Preliminary Off-Site Evaluation. Prior to


implementing the SAP, the Program Manager
and Health and Safety Supervisor should
review any Historical Overview and Site
Description sections of the SAP. This review
may result in the decision for an on-site
evaluation to assess the sampling procedures,
relevant safety equipment, and PPE.
Equipment Verification. The SAP should
specify an equipment list, including sampling
equipment, sample containers, and PPE. This
list should be reviewed in detail by the entire
sampling team and the Health and Safety
Supervisor to verify that necessary items are
included and appropriate for the site being
sampled.
Inventory. The Equipment Technician
(however named) shall gather all the specified
equipment and containers into one place and
verify that it is on hand. Reagents, supplies,
and quality control materials shall be checked
and verified as appropriate. The designated
technician shall notify the Program Manager
that equipment preparations are complete.

Chapter 3 Common Sampling Procedures

Sign-Over of Materials. The designated


individual shall check the equipment
inventory, and sign for custody if required.
Staffing and Scheduling. The Program
Manager shall consider the impact of specified
sampling requirements on staff and schedule.
Screening or Field Measurements. Sample
screening or field testing for pH, dissolved
oxygen (DO), sulfite, conductivity,
disinfection chemicals, and temperature
require additional field time. The need for
additional personnel is based on time
demands, training requirements and degree of
difficulty. Significant field testing
requirements may justify the procurement of a
field laboratory and a trained field chemist to
relieve other team members of this
responsibility.
Preservation. Preservation, either chemical
or thermal, is required for most water samples.
Thermal preservation usually requires icing
the samples after collection and storing
samples at 6 Celsius (C). For chemical
preservation, two practices exist for adding
preservative: 1) addition of the chemicals to
the samples in the field, and 2) addition of the
chemicals to the sampling containers prior to
sending the containers to the field. Adding the
reagents to the sample containers at the time
the samples are collected requires the sampler
to maintain records of addition and quality of
the reagents and to follow proper chemical
handling techniques. In some cases it may be
advisable to have the laboratory add the
reagents to specially labeled sample containers
before they are sent to the field. This may
reduce the fieldwork required and the
possibility of field error resulting from
contaminating the preservatives. Addition of
the correct amount of preservative can be
estimated for samples collected on a routine
basis having little to no outside environmental
or process effects.

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WARNING: When using containers filled with preservative, use caution when filling the bottles to ensure the
preservative is not released to the environment and the
correct amount of preservative has been added to adequately fix the sample.

Time. Many samples have short holding times


prior to analysis. Review the holding time
requirements and coordinate the schedule with
the laboratory so the samples are analyzed
within the required holding times. Holding
times are dictated by the regulatory program
and data may be invalidated if holding times
are not met.

Note: Refer to Appendix B of this handbook for specific


information on hold times, preservation, and containers.

3.2.1. Preparing for a Sampling Event


Preparing for a sampling event requires planning
and a thorough knowledge of the regulatory
program. The key elements for such preparation
include:

Objectives. The objectives should be


thoroughly understood by all sampling
personnel prior to sample collection.
Knowledge of the compliance scope,
boundaries, geography, and area roads and
bridges will facilitate sampling.
Map of Study Area. A map of the study area
is essential for sampling. The map should be
detailed enough so that sample locations and
landmarks are clearly identifiable.
Permits and Regulations. The person
collecting samples should have a working
knowledge of applicable permits, required
monitoring, and other specified conditions.
Regulations that potentially impact the
sampling area, such as right of entry, should be
reviewed by the sample collector.
Waste Sources. When the objective of a
project is to determine the nature, extent, or
impact of a waste source upon an
environmental medium, knowledge of waste
source(s) within the area, as well as those
sources upstream or upgradient that may
impact the area, is essential. This knowledge
entails knowing waste source discharge points
or areas, type of waste, volume of discharge,
Chapter 3 Common Sampling Procedures

and constituent concentration. When this


information is not readily available, it may be
necessary to collect background information.
Environmental Medium Characteristics. If
the study is of a waterway, the physical
characteristics of the waterway should be
known prior to sample collection. These
important physical characteristics include
whether the receiving waterway resembles a
lake, reservoir, pond, small stream, or a river.
Average and maximum recorded flow, width
and depth, type of benthic substrate, and type
of predominant aquatic vegetation also should
be noted.
If the study area is limited to land, it is
important to have knowledge of the terrain,
soils classification, geology, terrestrial
vegetation, industrial and residential
development, predominant land use, and
wildlife.
Sampling Information. A sampler must
know the types of samples to be collected,
(e.g., water, wastewater, soil, or solid waste).
The sampler also must know whether the
samples are to be collected nocturnally or
during the daytime, and where within the
environmental medium the samples are to be
collected (including both horizontal and
vertical collections) as well as the preferred
method of collection.
Laboratory Arrangements. Arrangements
must be made with the analytical laboratory to
ensure that the laboratory is expecting the
samples when they arrive and has a description
of the types of samples (e.g., liquid, semisolid, solid, or biological), an approximation
of the number of samples for each sample
type, and the analyses requested on each
sample type. Arrangements must be made for
the appropriate number of sample containers
and preservatives where required. Regulations
on transportation of samples from the point of
collection to the laboratory must be
considered, and the COC record must be
traceable, as detailed in the SAP.

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Equipment. Prior to going to the sampling


location, the sampling gear should be
examined to ensure that it is appropriate for
the task and in good working order. Verify
that any preventative maintenance has been
completed according to the SOPs. Label,
mark, and otherwise identify all equipment,
instruments, reference materials, and
associated supplies for measurement processes
to indicate calibration or standardization
status. Expiration dates of reagents and
solutions should be checked and verified as to
usability. If a boat is required, an appropriate
boat, motor, and life jackets must be available,
and preliminary boat launch locations should
be known before going to the sampling site.
All equipment should be examined prior to
starting the sampling event.

Note: When in use, sampling equipment should be anchored to prevent loss in the event the rope or equipment
slips through the hands of the sample collector.

Safety. The safety of sampling personnel is


paramount. During wading operations, a rope
should be attached to the sampler and
extended to an anchored person on shore. In
boating operations, at least two people should
be present, one to collect the samples and
another to operate the boat motor. Boat
personnel are required to wear life preservers
and take care to avoid overloading the craft.
When collecting samples, beware of snakes,
stinging insects, ticks, or other animals that
may cause injury to the sample collectors.
Personnel Transportation and Lodging.
The Program Manager must consider
arrangements for transporting sampling
personnel and equipment to the sampling site,
and for lodging when the sampling extends
beyond a working day.
3.2.2. Preliminary On-Site Evaluation
When sampling for the first time at a new location, a preliminary on-site evaluation should be
conducted prior to the sampling event to ensure
that all aspects of the sampling process are addressed.

Chapter 3 Common Sampling Procedures

Upon arrival at the site, the Program Manager (or


designee) and the Health and Safety Supervisor
shall check with facility personnel to determine
whether there have been any recent changes at the
sampling locations that would influence the SAP
or modify the expected hazards.
3.2.3. Preliminary Site Safety Evaluation
After a preliminary hazard analysis, sampling
locations should be inspected to develop the
Safety Plan or HASP as appropriate to the scope
of the project. PPE information specified may
not be completely reliable, and additional air
monitoring may be required. When air monitoring activities are needed, focus first on identifying conditions that present an acute health hazard,
and then evaluate exposure to chemicals such as
carcinogens that could create long-term health
problems.
If samples are to be collected in a confined spot,
testing the air within the space for oxygen content
should be a priority. Tests for explosive levels of
flammable vapors should be conducted next,
followed by testing for the presence of hazardous
concentrations of specific toxic agents (depending
upon the nature of the space and its contents or
previous contents).
Note: Real-time instrumentation is available for making
these measurements. Air samples should be collected to
evaluate the levels of other chemicals in the air that may
require respiratory protection. Some organic chemicals
such as gasoline vapors can be monitored with standard
field instruments. However, monitoring for carcinogens
will normally require the use of a field gas chromatograph
or the collection of test samples for laboratory analysis.

In general, the air monitoring program to evaluate


worker exposures to toxic chemicals should be
designed by an industrial hygienist familiar with
the facility and potential hazards to which the
field sampling team will be exposed.
Review physical hazards that may be present at
the site, such as unstable footing near river embankments, water safety practices, first aid supplies, equipment safety practices, and other physical hazards.

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3.2.4. Explosive Safety Evaluation


The possibility of encountering explosive hazards
must be considered in all sampling plans. When
the presence of energetic materials is suspected
from the history of a site, appropriate precautions
can be incorporated during the planning stages.
Consideration should also be given to situations
that can lead to the formation of unstable materials from constituents that are not originally
energetic compounds. Formation of peroxides in
ethers and metal picrates are two examples that
have been known to create safety hazards.
3.2.5. Preliminary Sampling Evaluation
Sampling locations should be inspected to ensure
the information in the SAP is correct. All equipment should be checked prior to mobilization and
the day before the sampling event to ensure proper equipment operation, parts, and records are
available for the sampling operation. If needed,
preventative maintenance should be performed.

Reagents, supplies, reference materials, and


consumable materials should be verified as to
expiration dates, quality, and applicability to the
assigned equipment.

Locate all the sample locations during the on-site


evaluation to determine site accessibility with the
designated equipment, sample location, and
possible background contamination for the contaminants of interest. Electromagnetic interferences, volatile air pollutants from locations off
site, weather, and climate may affect the sampling
event and should be planned for, as much as
practical, to avoid delays in sampling.

3.3.

The Sampling Event

A typical sampling event should include the


following sequential activities:

Complete all preparation and preliminary


evaluation activities as needed
Arrive at the sampling site with appropriate
equipment, supplies, materials, and sample
containers
Set up equipment, work areas, and safety
areas, as described in the SAP
Chapter 3 Common Sampling Procedures

Collect samples at the locations specified in


the SAP or reference procedure
Immediately following sample collection,
ensure that each sample container is labeled as
described in the SAP. The sample label must
be traceable to the sample number, date/time
sampled, samplers name, preservative, and
site name, location or unique project identifier.
Document the exact location of the collected
sample(s) in the field logbook or field
notebook (FLB/FN). Also, record in the
FLB/FN other observations of environmental
conditions that could affect or contribute to
knowledge of the sampling area and the
environment where the sample is collected.
Prevailing weather conditions at the time of
sampling should also be recorded.
Preserve or ice samples as appropriate and
record preservation method
Perform field tests or field screening measurements and record all observations in the
FLB/FN
Complete the COC record and other field
records
Pack and seal the shipping container with
collected samples, and transport the shipping
container with the COC record and any
laboratory required forms to the laboratory.
Retain copies of all transmitted forms.
Return all forms and copies of relevant
FLB/FN pages to the Program Manager or
designee
Clean sampling equipment for the next
sampling event or storage
Breakdown all work area and safety areas as
required and return the site to the condition
found at the start of the sampling event
Dispose of all waste materials using
appropriate procedures.

3.4. Sampling Procedures


The SAP refers to detailed sampling procedures
or includes the details of the sampling operation.
A standard SOP format should be used to incor-

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porate the following items for each type of sampling operation:

Sampling locations, sample numbers or


identifiers
Type, volume, and number of sample
containers to be filled at each sampling
location and the records to be maintained
Contaminants to be measured and special
handling procedures to ensure proper
collection
Safety, health, and hazard cautions
Sampling equipment (construction material,
type, etc.) and records to be maintained for
status, maintenance, and corrective action
Step-by-step sample collection procedures
(grab, composite, continuous for specified
period, etc.)
Sampling frequency for repeated sampling at
the same sample location
Special sampling requirements (e.g., the
collection of initial runoff samples after a rain
for contamination)
Sample handling procedures for each sample
container (e.g., screened, filtered, sequence for
filling groundwater sample containers, etc.)
Preservatives required for each sample
container and contaminant
Reagents, supplies and support services
quality, verification and validation criteria to
ensure materials are used properly
Equipment decontamination procedures to be
used between sample locations and between
sampling events
Recordkeeping requirements, documentation
handling, and retention requirements
Sample, equipment, and materials storage
requirements
Provisions for storage or disposal of wastes
generated during field sampling.

3.4.1. Sampling Strategies


See Appendix A for sampler and sampling recommendations and strategies for waste materials.
Sampling strategies for drinking water, wastewaChapter 3 Common Sampling Procedures

ter, groundwater and TSCA materials are permit


or compliance dependent. The Scope or Purpose
section of the sampling procedures should describe the rationale for the sampling strategy to
ensure that all personnel involved with the project
have an understanding of the sampling event.
3.4.2. Sampling Procedure Checklist
Following is a checklist of the minimum steps to
address in SOP format.

Sampling Approach
- Objective
- Design of sampling plan
- Statistics
Material to be Sampled
- Physical state
- Volume
- Hazardous properties
- Composition
Site
- Accessibility
- Waste generation and handling
- Transitory events, startup, shutdown
- Maintenance
- Climate
- Hazards
Equipment
- Maintenance
- Preparation and cleaning
- Operation
- Calibration and standardization
Sample Handling, Transportation, Storage
and Preservation
- COC
- Seals
- Forms
- Containers
- Preservatives, reagents, and supplies
QA/QC
- Controls on process
- Audits
- Training
- Samples, blanks, duplicates, and
spikes
Health and Safety
- Personnel protection
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- Safety procedures
- Emergency procedures
Laboratory
- Document transfer
- Sample arrival schedule, transfer
- Sample preservation, handling and
storage
- Analytical methods and QC
- Reporting format and schedule.
3.5. Sample Documentation and COC
Procedures
Thorough documentation of a samples custody is
required to support sample validity. The documentation must verify that the samples are representative, were collected in accordance with the
requirements of the SAP, and are not vulnerable
to tampering before being received by the laboratory. The COC begins when the sample is taken and
ends when the sample is disposed of. Sample
documentation and COC procedures include the
following.
A completed sample collection label attached to
all sample containers
Records of sampling operations written in
FLB/FN or related forms as designated for the
operation in the SAP. Records include sample
type, sample matrix, sampling method, field test
methods, and QC procedures. A table may be
used to present this information.
Identification of every sample container on a
COC record and all custody transfers
documented
Custody of the samples with all discrepancies in
the field operations resolved or duly recorded.
The following should be used to generate the required sample documentation.
________________________________________
Note: EPAs Field Operations and Records Management
System II Lite (FORMS II LiteTM) software is an electronic COC and may also be used to simplify and accelerate the
sample documentation process.

3.5.1. Pre-Assigned Sample Numbers


Each sample consists of all of the material collected
for analysis at one place, at one time, and of one
Chapter 3 Common Sampling Procedures

matrix, except for composite samples, which may


contain components collected at different locations
or time.
The Program Manager shall establish a system for
assigning a unique sample number to each sample
collected in the field. The numbering system will
be defined in the SAP, in case additional samples
are generated in the field. The number for each
sample will be used to identify the sample in the
FLB/FN, on the sample container, and on the COC
record. The number may be used on other forms
and reports presenting measurements, test data, or
evaluations.
The sample numbers of field QC samples like a
field duplicate should be transparent to the laboratory. The sample numbers should not reveal
whether a sample is a blank sample or two field
samples are duplicate/split pairs to avoid potential
biasing of analytical results.
The sample number provides a common identifying
code for all of the analytical results for a single
sample. This is particularly useful when the results
are entered into a computer database, which should
include:
Sample number
Sample container number
COC record number
Matrix
Location
Sample type
Sample date and time
Samplers name
Parameter
Analytical result
QC data
Compliance limit and
Data qualifier code (optional).
Results from analysis of trip blanks, field blanks,
equipment decontamination blanks, split samples
and MS/matrix spike duplicate (MSD) samples
may be entered into a computer database. In
some testing programs, these results are used to

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generate the data qualifier code for the analytical


results from test and duplicate samples.
It is recommended that the information associated
with each sample number consists of elements
describing the sample type, matrix, location, and
the time and date of sample collection as required.
Note: If the sampling and analytical data are to be added to
an existing database, sample numbers should be consistent
with database requirements.

Note: Because 40-mL volatile organic analysis (VOA) vials


may be stuck in an autosampler, the field sampling team
leader needs to contact the laboratory to make sure if
applying a clear tape over a sample label of 40-mL VOA
vials is acceptable. Use waterproof ink to make label
entries. FLB/FN notations should provide an explanation if
a pencil was used to fill out the sample container label due
to field weather conditions. Because waterproof ink may
contain target VOAs such as xylene, toluene, or alcohols as
a solvent, great care is needed to prevent VOA samples
from contamination by the solvent of waterproof ink or
permanent marker.

Figure 3-1. Multiple Part Container Label

3.5.2. Sample Container Labeling


Sample labels are an important part of proper
documentation to reduce the possibility of confusing sample containers, and to provide the
necessary handling information. Sample containers should be pre-labeled as much as practical
before sample collection. The labels may be
protected from the sample matrix with a clear
tape covering. For volatile samples, check with
the laboratory to ensure that any labels being used
do not interfere with their auto-samplers. Sample
labels should include sample number, date and
time sampled, location, sample type, preservative
and the samplers initials or signature.
Sample numbers may be unique to the sample
location, to the sample type or to the container.
In some labeling processes, a unique sample
number is written on the container label, and all
information recorded on the accompanying
form(s) is traceable to the unique sample number.
Some number schemes uniquely number each
sample container. All data reported for the sample includes the sample container number for
traceability to the container measured. This is
useful when sample containers are cleaned and lot
controlled, and traceability from container preparation, preservation, sampling, and testing is
required.
A designated Field Sample Custodian or sampler
should label the sample containers when they are
filled. Preprinted, adhesive, multiple part labels
formatted as shown in Figure 3-1 may be used.
Each part includes the unique sample container
number that may be pre-numbered to avoid duplication.
Chapter 3 Common Sampling Procedures

PROJECT NAME
Sample #: XXXXX
Container #: XXXXX
Sample #:
_______________
Date: ______
Time: _________
Location:
________________
Cont. Size:
________________
Cont. Type:
________________
Matrix:
________________
Type of Sample: _______________
Preservative:
________________
Signature:
________________
3.5.3. FLB/FN
The FLB/FN is the written record of all field data,
observations, field equipment calibrations, and
sample collection activities. Potential for future
legal actions dictates that the FLB/FN be sitespecific and that they be hardbound (e.g., ledger,
composition book, diary, etc.). All pages (front
and back) shall be serially numbered so removal
will be apparent. Samplers shall adhere to the
following guidelines when using FLB/FN.

The FLB/FN shall be assigned to the QA/QC


Coordinator or designee. Additional log books
may be assigned by the Program Manager or
designee to the Field Chemist and the Health
and Safety Supervisor. The QA/QC
Coordinator or designee shall note in each
FLB the individual to whom it was assigned.
The FLBs may be controlled by the QA/QC
Coordinator or the Program Manager.
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Each FLB shall be annotated with the


sampling program name or number.
Key personnel and telephone numbers shall be
listed on the first page.
Entries shall be written in waterproof blue or
black ballpoint pen. Avoid felt tip pens. Do
not use pencil.
Start a new page at the beginning of each day.
Entries should be chronological a time
notation should introduce each entry.
Sketch or obtain a map of the area or facility.
Include sketches of layout, structural features,
and points of interest or contamination.
Include a north arrow and a rough scale. If
possible, obtain a site map (reduced if
necessary) and permanently place it in the
FLB/FN.
Language should be objective, factual, and
free of personal feelings or other inappropriate
terminology. Speculation or personal
observations may be included if they are
clearly identified as such.
Do not erase or scratch out errors. Draw a
single line through the error, then insert
corrected material. The person who made the
error shall initial and date the correction as
well as clearly state the reason for the error.
Entries or corrections made by individuals
other than the person to whom the FLB/FN
was assigned shall be signed and dated by the
individual making the entry or correction. An
explanation for the correction should be noted.
The last entry for each day should include a
short summary of the days activities, weather
conditions and the time the site was left. As
appropriate, the last entry for each week
should be a summary of the weeks activities.
Weekly summaries should be thorough and
descriptive.
The FLB/FN shall be signed at the end of each
day. Signatures shall be written on a single
diagonal line drawn across the blank portion of
the page following the days last entry.
All FLBs/FNs shall be returned to the
individual designated for review and final

Chapter 3 Common Sampling Procedures

storage when sampling is completed as


described in the SAP.
FLB/FN entries will contain a variety of
information. Information to be entered at the
start of each day of sampling includes the
following:
- Date of the sampling event
- Time sampling started and
approximate time for set up of
equipment
- Weather conditions
- Level of PPE being used
- Names of field sampling team
members and others present during the
sampling.
Fully document all deviations from the SAP or
changes in sampling procedures. Problems,
delays, or any unusual occurrences such as
improper equipment or breakdowns should be
included, along with resolutions and
recommendations. Summarize the content and
conclusions of all relevant meetings,
discussions, and telephone conversations in
which you are involved. Include the names
and affiliations of all personnel involved.
Thoroughly document all directives and/or
guidance from EPA or other government
personnel. Directives that give personnel
specific authority to make critical decisions
must be documented in the FLB/FN.
Whenever a sample is collected or a
measurement is made, a detailed description of
the location must be recorded. The source
from which the sample is collected should be
clearly identified to maintain traceability and
allow another person to locate the exact
sampling location. The ability to relocate the
sample site ensures duplication of future
sampling events. Measurements from
permanent features (e.g., center line of road,
numbered utility pole, etc.) to the sample point
must be made and entered into the FLB/FN.
Coordinates on a map, or an accurate site
sketch with distance measurements to known
locations are other options to ensure the exact
location of each sample is recorded.

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Describe the site thoroughly so another person


will be able to locate the exact sample location.
Note signs of contamination such as oily
discharges, discolored surfaces, unusual odors,
dead or distressed vegetation including types of
plants, if possible. Photographs may be taken to
provide evidence of visual observations, record
site conditions, and assist with locating the
sample site in the future. Photographs taken of
sample locations should be noted along with the
picture number. Log the record in the FLB/FN
to identify which sampling site is depicted in the
photograph.

Note: A series of photographs can be identified by taking


the first photograph of an informational sign with the
sampling program name, number, and the project number
on it.

Each time a sample container is filled and


labeled, a copy from the multiple part form of
the sample container label or reference number
label with all information recorded shall be put
into the FLB/FN.
All equipment used to make measurements
must be identified by type, manufacturer, and
serial number, along with the date of
calibration. Details of field calibration
procedures and results shall also be included in
the FLB/FN.
Note decontamination or disposal procedures
for all equipment, samples, protective clothing,
and personnel decontamination procedures.
For each delivery or shipment of samples to a
laboratory, record the following information in
the FLB/FN:
- Custody procedures and serial
numbers
- Packing and shipping procedures
(record air bill numbers)
- Name, address, telephone number, and
contact of the laboratory performing
the analysis.
Note: The laboratory address should be the sample receipt
address, which may not be the same as the mail receipt
address.

Chapter 3 Common Sampling Procedures

3.5.4. Field Notes/Field Sampling Forms


Field notes or field sampling forms are used in
addition to or in lieu of field log notes. When
field notes are used in lieu of an FLB, the record
keeping practices presented in Section 3.5.3
should be followed. The field form provides a
place for the sampler to record the information
required for the project. Field forms are specially
designed for any given project and may be completed one per sample or one per sampling event.
The forms include blank lines for recording the
information necessary for the project to ensure
the proper information is recorded. All blanks
must be completed on a field form to ensure
proper documentation. The sampler completes
the field form for all samples collected including
QC samples. An example of a field form for a
well sampling activity is presented in Figure 3-2
below.
Note: A review of the regulatory programs specific requirements must be conducted to ensure that all documentation requirements are met. Some programs do not allow the
use of loose field forms as the sole documentation vehicle
and require hardbound logbooks.

The field form lists the sample number, location,


matrix, the type and number of sample containers
filled (including QC samples), any chemical
preservatives added and checked for each sample
container, sampling procedure reference, deviations to the procedures and all field measurements
and observations.
The Field Sample Custodian indicates acceptance
of the information on the field form by signing
and dating the form. In cases where multiple part
forms are used for the sample label, for each
sample container filled, one part of the multiple
part adhesive sample container label is placed on
the field form at the appropriate location. The
completed field forms are returned to the Program
Manager as soon as possible and by the means
indicated in the SAP. Deviations or problems
encountered during the sampling event must be
communicated promptly in writing to the Program Manager or designee. This may be completed by sending the field form by facsimile or
other means to communicate the deviations, as
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well as allow for continuation of the project and


ensure sample holding times are not jeopardized.
Note: The field form becomes part of the permanent project
records, but is not usually sent to the laboratory.

3.5.5. Chain of Custody (COC)


An overriding consideration for environmental
measurement data is the ability to demonstrate that
samples have been obtained from the locations
stated and that they have reached the laboratory
without alteration. Documentation of security,
field handling criteria, shipment, laboratory receipt, and laboratory custody until disposal, provides evidence of proper processing. The degree
of custody documentation is dependent on the
regulatory program, data use, and needs. Many
state programs for sampling wastewater and drinking water do not require legal custody, but recommend legal custody whenever data is known to
be used for evidence. A review of data use and
risk of legal proceedings will dictate the type of
custody procedure to be employed. Documentation consists of a COC record that is completed by
the Sample Custodian.

Chapter 3 Common Sampling Procedures

3.5.5.1. Field Custody Procedures


The Field Sample Custodian or sampler is personally responsible for the care and custody of the
samples until they are transferred or properly
dispatched. As few people as possible should
handle the samples. A sample is considered to be
in custody for legal proceedings if it is:

In a persons actual possession


In view after being in physical possession
Locked up so that no one can tamper with it
after having been in physical custody
In a secured area, restricted to authorized
personnel only.
If any one of these is not in place at all times, the
COC is broken.
The Program Manager or designee shall review
all field activities to determine whether proper
custody procedures were followed during the
fieldwork and whether additional samples are
required. The sampler or Sample Custodian shall
notify the Program Manager of any breach or
irregularity of COC procedures described in the
SAP.

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Figure 3-2. Field Form


MICROPURGE/LOW-FLOW SAMPLING LOG

Sheet _1__ of __1_

PROJECT:
EPA ID NO:
Proj./Task No.
Date:
Weather:
Samplers:

WELL ID:
Well Condition:
Well Riser Dia. (ID):
Screened Interval:
S.W.L. Measuring Pnt:
Well Bottom Depth:

Purge Method: Micropurge


Sample Collection Method:
Sampling Device:
Pump Intake Depth:
Tubing:
Total Recovered Purge Water This Well:
Groundwater Sample Data:
Sample ID
Analysis
Primary

QC

STATIC WATER LEVEL:


Initial Purge Volume:
Approximate Pump Throttle Setting:

MS/MSD

Blank

Instrumentation/Equipment Data:

Sample ID

Analysis

Primary

QC

MS/MSD

Calibration Date:

Field Test Results:


Hach Kit Tests:
D.O.
Total Iron:
Ferr. Iron:
CO2:
Comments:
Observations: Clarity:
Odor:
PURGE WATER DATA TABLES
Stabilization
Parameters
Units
Minutes Minutes Minutes Minutes
Temperature
C
Sp. Cond.
ms/cm
D.O.
ppm
pH
ORP (Eh)
mV
Turbidity
NTU
Clock Time
Static W.L.
Flow Rate
ml/min.
Stabilization
Parameters
Temperature
Sp. Cond.
D.O.
pH
ORP (Eh)
Turbidity
Clock Time
Static W.L.
Flow Rate

Units
C
ms/cm
ppm

____
Minutes

____
Minutes

____
Minutes

____
Minutes

mg/L
mg/L
mg/L
mg/L

Floating Product:

Sheen:

Minutes

Minutes

Minutes

Minutes

____
Minutes

____
Minutes

____
Minutes

____
Minutes

mV
NTU

Chapter 3 Common Sampling Procedures

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3.5.5.2. COC Records


From time of collection through final sample
disposal, there are many transfers of custody
during the course of a sampling program. All
sample containers must be accompanied by a
COC record to document these transfers. A
separate COC record shall be prepared by the
Field Sample Custodian or sampler for each
sampling event. In some programs, a COC
record accompanies each shipping container and
includes a pre-numbered COC record. This
record lists the sample containers that are in the
shipping container, and serves as the packing list
for the container. The serial number on the form
becomes the identifying number for the shipping
package.
Figures 4-3 provides an examples of a sample
COC record. The example has been used for a
wide variety of regulatory programs and meets
legal COC requirements. It tracks the samples
from sample collection to disposal. All sampling,
preservative, and test information is included.
The SAP will indicate the individual responsible
for completing each section. The following
information relates to the numbered blocks:
COC RecordFigure 3-3.
(1) The company/command name and code for
the source of the funding.
(2) The contact name for the Program Manager
or designee indicated in the SAP.
(3) The job order number (J.O. #) is entered
to trace the information to the specific job.
(4) The signature of the Program Manager or
designee authorizing the funds.
(5) The permit number (No.), if applicable, for
the samples collected. The number is issued
by the regulatory agency for specific compliance reporting.
(6) The sample ID/location based on permit
designations or actual site location name.
(7) The sample taken date and time are recorded for grabs on the start line only and for

Chapter 3 Common Sampling Procedures

composites on the start date and time and


stop date and time.
(8) The code for sample type such as grab,
composite flowing and composite time (see
Section 18).
(9) The initials for the person sampled by.
(10) The code for sample matrix such as liquid,
solid, and gas (see Section 18).
(11) The code for preservative (see Section 18).
(12) The # of samples and container type are
entered as 4-P for four plastic containers
(See Section 18).
(13) The analysis to be performed - may reference descriptions in the SAP.
(14) The field reading for pH for the sample
containers indicated.
(15) The field reading for temperature with the
unit of measure for the sample containers
indicated. The SAP may indicate the temperature to be recorded in the outfall temperature and not the sample temperature.
(16) The field reading for other required measurements may be entered with the unit of
measure. The SOP and name of the test
must be indicated on the custody form.
(17) After the samples are preserved, the preservation is verified. The verification is noted
per the SAP. This verification may be temperature, pH, or if all is correct an indication
is made as OK.
(18) This section of the custody form contains
common codes to be used by the sampler
when completing the custody record. When
situations arise that do not match the code
designations, alternates may be added for
the one time use on the custody form.
(19) The expected turnaround for sample request is placed in this area. The reason is
presented to determine if the turnaround
time is regulatory, project specific, or based
on holding time requirements.

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(20) Special instructions or comments may be


entered in this space.
(21) The regulation applied to the project is
checked.
(22) The sample collection/charge, possible
sample hazard and other comments relate
to the command in charge of sampling, special sample hazards, or to other sample
comments. Reference may be made to code
or specific sections of the SAP.
(23) The delivery order number is entered.
(24) The contract lab and contract number
(No.) are entered for testing work performed
by a designated contract laboratory.
(25) The sample disposal method and the date
completed.
(26) The signature and company/command of
the person relinquishing custody (relinquished by).
(27) The signature of the person custody is received (recd) by.
(28) The date/time custody is transferred.

Chapter 3 Common Sampling Procedures

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Figure 3-3. COC Record

Chapter 3 Common Sampling Procedures

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The COC record identifies which pairs of sample


containers were collected for the same analysis,
and identifies the sample containers that were
filled with sample for use as the MS/MSD QC
samples. Based on the needs and data use, the
COC record may not list any information as to the
exact sample location or whether a sample is a
field duplicate, field blank, trip blank or an
equipment decontamination blank. This information is kept as blind information from the laboratory to ensure objective reporting. When this
process is used, records must be maintained that
trace the sample collected in the field with the
sample as identified to the laboratory. Compliance data for drinking water or wastewater
testing do not require blind submissions. The QC
sample information is provided to the laboratory
to ensure prompt notification when the QC data
does not meet the SAP specifications.
Whenever samples are split with a second laboratory or government agency, a separate COC
record may be prepared for the second set of
samples. The additional set of COC records must
be noted. Copies of the original may be sent with
the split samples noted, or a separate form may be
prepared by copying the appropriate information
for the samples onto the additional form. In all
cases, the use and need of the additional form
should be noted.
Upon completion of the packing of each shipping
container, the Field Sample Custodian shall confirm the completeness of the COC record by
signing the COC record. If a multiple-part form
is used:

The original copy is put into the shipping


container
The first copy is sent immediately (preferably
by fax) to the Program Manager or designee
The second copy is kept with the FLB/FN or
copy of the field form.
If a single part form is used, photo copies should
be made for the Program Manager and the FLB.
After the COC record is completed and all samples are packaged and shipped to the appropriate
locations, the person relinquishing the samples to
Chapter 3 Common Sampling Procedures

the laboratory or agency shall request the representatives signature acknowledging sample
receipt. If the representative is unavailable or
refuses to sign, this is noted in the received by
space.
Field COC terminates upon laboratory receipt of
the samples. The laboratory should complete the
received by sections and if appropriate, the
preservative checks sections on the COC record
and return the original signed record to the Program Manager. If there are any discrepancies
between the COC record, the contents of the
shipping container, and the SAP or contract
requirements provided to the laboratory, the
samples in question shall be segregated from
normal sample storage, and the laboratory shall
immediately notify the Program Manager. In
some cases, the laboratory checks the sample
submittal and recordkeeping to ensure adherence
to the SAP. This added check is often used in
drinking water and wastewater testing programs
for compliance monitoring. Recordkeeping and
information checks should be performed by the
laboratory to ensure the samples received meet
the requirements of the SAP.
3.5.5.3. Custody Seals (Optional)
Custody seals are narrow strips of adhesive paper
used to indicate whether a shipping container has
been opened during shipment. The seals are
placed along the edges of the most exterior container in which samples are enclosed. It is not
always necessary to place seals on individual
sample containers in the shipping container.
Paper custody seals should be signed and applied
before the shipping container is shipped to the
laboratory. The preferred procedure includes use
of a custody seal attached to the front-right and
back-left of the container. Custody seals are
covered with clear plastic tape. Another way to
use custody seals, is to put all sample containers
with packing and ice in a large garbage bag and
seal the garbage bag with a signed custody seal.
3.5.5.4. Custody Transfer
Transfer of custody and shipment procedures are
as follows.
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Each sample shipping container shall be


accompanied by a properly completed COC
record. The original of the record shall be
included in the container. The Field Sample
Custodian shall keep a copy of the completed
form as part of permanent documentation and
will send a copy of the COC record to the
Program Manager.
When transferring possession of samples,
individuals relinquishing and receiving shall
sign, date, and note the time of the transfer.
This record documents custody transfer from
the Field Sample Custodian to another person,
to a mobile laboratory, to the permanent
laboratory, or to a secure storage area.
If the sample container is sent by common
carrier, a bill of lading shall be used. Bill of
lading receipts shall be sent to the Program
Manager for permanent retention. If sent by
mail, the package shall be registered with
return receipt requested. Commercial carriers
and the U.S Postal Service are not required to
sign off on the COC record as long as it is
sealed inside the package with the sample
container and the custody seals remain intact
(if used).
3.5.6. Request for Analysis
The Request for Analysis form is often incorporated into the COC record since the chain must
accompany the samples. In more complex sampling programs, an additional form may be used
to request testing.
When contracting for laboratory services and
prior to submitting the samples, the laboratory
should be contacted and the following information presented. The Request for Analysis form
can be used as a preliminary contact mechanism
to ensure that the scope of work is understood.
This form:

Specifies the analyses, procedures, and QC


data to be performed on each sample container
and the compliance protocols to be followed
Specifies the laboratory accreditation/
certification required to be maintained during
the period of the contract
Chapter 3 Common Sampling Procedures

Authorizes the payment for the analyses


Alerts the laboratory to any anticipated
hazards associated with the samples and
custody procedures to be followed while the
samples are in the possession of the laboratory
Specifies the reporting requirements and
content for the final report from the laboratory
Instructs the laboratory as to the disposition of
the samples after the completion of the
analyses.
3.6. Sample Packaging, Handling, and
Transportation
The Field Sample Custodian is responsible for the
proper field storage, security, packing, and shipping of the samples from the field to the laboratory or designated holding location. The packaging, labeling, and shipment of samples by common carrier are regulated by the DOT and the
International Civil Aviation Organization
(ICAO)/International Air Transport Association
(IATA), when appropriate. Instructions for classification, labeling, and packaging of hazardous
materials are contained in DOT regulations
(49 CFR 172 and 173, and subsequent Parts).
Overnight couriers generally accept materials
shipped under these regulations. However, some
couriers have additional restrictions for hazardous
shipments. EPA also regulates the shipment of
hazardous waste and hazardous material by requiring labeling on certain packages.
The procedure for determining whether a sample
is hazardous under DOT regulations is complex,
as is the determination of the proper shipping
name, packaging requirements, and labeling
requirements for DOT hazardous materials. A
summary of specific requirements are addressed
below. Should questions arise, assistance is available from the DOT (1-202-366-4000) and Federal
Aviation Administration (FAA)
(1-866-835-5322) hotlines.
Samples obtained at sites are classified for shipping purposes as either environmental (nonhazardous) samples or hazardous samples. If a
material is being shipped for testing to determine
its hazards, a tentative hazard class assignment
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should be made based on knowledge of the material. Samples requiring special packaging or
labeling are those containing chemicals that are
listed as hazardous materials in:

49 CFR 172.101
CERCLA RQ Hazardous Substances
DOT CLASS 9 listed in 49 CFR 172.101
Appendix A, Poison DOT Class 6.1 and
Flammable Liquids.
Environmental (non-hazardous) samples are those
that are not classified as Hazardous Materials
under DOT regulations, are packaged in quantities less than the CERCLA RQ, and for which a
Hazardous Waste Manifest is not required by
EPA. These samples require careful packing, but
no special shipping procedures. In general, samples of groundwater, surface water (other than
leachate or lagoons), and soil may be shipped as
environmental samples (non-hazardous) to an
analytical laboratory for testing if each of the
sample containers contains less than 1 pound of
soil or 1 gallon of water, and the entire shipping
package weighs less than 66 pounds. Eventual
analysis for a hazardous constituent does not
necessarily classify a sample as a DOT hazardous
material, nor does the classification of a material
as a hazardous waste under EPA regulations.
DOT regulations forbid the shipping of nonhazardous materials as hazardous. However, if
any doubt exists as to whether the sample might
be classified as a hazardous material, the sample
should be treated as hazardous.
Note: For details on the shipping of non-hazardous waste,
refer to ASTM D6911-03: Standard Guide for Packaging
and Shipping Environmental Samples for Laboratory
Analysis. This standard provides guidance in determining
the most appropriate procedures for packaging and shipping
environmental samples.

The storage and disposal of hazardous waste is


regulated by the EPA. Hazardous waste, as
specified in 40 CFR 262, is not exempted from
EPA manifesting requirements. However, EPA
RCRA regulations exempt samples collected for
analysis or treatability testing from the RCRA
requirements that otherwise apply to hazardous
waste (including the requirement for a Hazardous
Chapter 3 Common Sampling Procedures

Waste Manifest). The definitions for these exemptions are:

Samples for Analysis. 40 CFR 261.4(d):


Samples of solid waste, water, soil, or air,
which are collected for the sole purpose of
testing to determine their characteristics or
composition, when samples are being sent to
the laboratory for testing or are being returned
to the collector after testing.
Samples for Treatability Testing.
40 CFR 261.4(e): Samples collected for the
purpose of conducting treatability studies
when they are being transported to the testing
facility provided they meet criteria for the
quantity of material, packaging, and permit
status of the receiving facility.
3.6.1. Sample Packaging Requirements
The Field Sample Custodian is responsible for the
packing and shipping of the samples from the
field to the laboratory. Samples shall be properly
packaged for shipment and dispatched to the
laboratory for analysis with a signed custody
record enclosed in the shipping container box or
cooler. Shipping containers shall be locked or
secured with strapping tape in at least two locations. Shipments that are sent to an on-site laboratory or one in close proximity that does not
require the use of a common carrier shall be
transferred in accordance with local regulations.
Table 3-1 below lists sample packaging procedures that will ensure samples arrive at the laboratory with the COC record intact.
The following major issues must be addressed in
preparing environmental samples for shipment to
the laboratory by common carrier:

Compliance with EPA regulations, so the


samples are not classified as hazardous waste
Compliance with transportation regulations,
including use of the proper shipping
containers, use of warning labels, and
completion of the required paper work
Packing, to assure that the samples do not
break or leak during shipping. This includes:

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- Using approved containers meeting


DOT drop test specification
- Lining coolers or containers with
plastic bags
- For glass containers, wrapping each in
bubble wrap and placing in a clear
plastic resealable food bag
- For plastic containers, placing each in
a clear plastic resealable food bag
- Never stacking glass containers or
laying glass on its side.
3.6.1.1. Samples Classified as Flammable
Liquid
Table 3-2 Column 1 lists packaging procedures
that apply to those flammable and combustible
liquids that do not meet the definitions of another
hazard class except DOT Class 9, and for which
exceptions under 49 CFR 173.150 are allowed.
This includes Flammable Liquids Not Otherwise
Specified (NOS), toluene, gasoline, and many of
the other flammable liquids that are commonly
encountered on hazardous waste sites.
Note: The DOT definition of liquid is different from that
used by EPA. For purposes of transportation, liquid means
a material that has a vertical flow of over 2 inches (50 mm)
within a 3-minute period, or a material having 1 gram or
more liquid separation, when determined in accordance
with the procedures specified in ASTM D4359-90, Standard
Test Procedure for Determining whether a Material is a
Liquid or Solid, (49 CFR 171.8).

3.6.1.2. Samples Classified as Poison


DOT Class 6
Table 3-2 Column 2 lists packaging procedures
that apply to those poisonous liquids and solids
for which exceptions under 49 CFR 173.153 are
allowed. This includes 1,1,1-trichloroethane,

Chapter 3 Common Sampling Procedures

trichloroethylene, trichlorobenzene, PCB transformer oil, and many of the other poisonous
materials commonly encountered.
3.6.1.3. CERCLA Reportable Quantities
DOT Class 9
Table 3-2 Column 3 lists packaging procedures
for substances (liquids and solids) where the
waste material is not otherwise classified as a
DOT Hazardous Material because of hazardous
properties and for which the entry in Column 8a
of 49 CFR 172.101 Table is 155. For the shipment of larger quantities of EPA hazardous waste
and DOT Class 9 hazardous substances where the
quantity of material in each container exceeds the
CERCLA RQ and no other DOT Hazardous
Material classification applies, the following
packaging requirements apply:

Label each container with a separate container


number
Seal each drum or pail with a Security Seal
Prepare one COC record for each group of
containers that is being shipped at the same
time to the same destination. List the
container numbers on the COC record.
These shipments may include EPA Hazardous
Waste in 5-gallon cans and 55-gallon drums. Most
DOT containers are approved. The list of approved containers for packing Groups II and III
Class 9 Hazardous Substances are listed in
173.203 for liquids and 173.213 for solids.
These lists include steel, aluminum, plastic and
fiber drums (solids only). Quantity limitations are
shown in 49 CFR 172.101, Column 9.

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Table 3-1. Packaging by Common Carrier


By Common Carrier
Instructions

Nonhazardous
Samples

Hazardous
Samples

Secure sample container lids with strapping tape.

1*

1*

Mark the level of material in each sample container with a grease


pencil.

Place each container in a clear plastic resealable food bag so that


the sample container label can be read.

Place about inch of inorganic cushioning material such as


vermiculite in the bottom of a metal can.

Place each container in a separate can and fill the remaining


volume of the can with an inorganic cushioning material such as
vermiculite (do not use plastic foam cushioning material as it
could dissolve if the sample container were to leak).

Close the can using three clips to secure the lid.

Write the sample number on the can lid. Indicate This Side Up
by drawing an arrow on the can.

Put about 1 inch of cushioning material (e.g., vermiculite or


plastic foam) in the bottom of a watertight metal or equivalent
strength plastic shipping container. If the container is a cooler,
seal the drain plug on the inside of the cooler with tape. Also line
the inside of the container with a plastic bag.

Wrap glass bottles and jars in plastic bubble wrap.

Place cans in the container and fill the remaining volume of the
shipping container with packing material. Add ice bags if
required.
Place the sample containers top-up in the shipping container.
Arrange the sample containers so that glass containers are
surrounded by plastic containers.

Fill the void space around and on top of the sample containers
with plastic bags filled with ice cubes or ice chips.

Seal the COC record in a clear plastic resealable food bag and
tape it securely to the inside of the shipping container lid.

10

Close and lock or latch the shipping container.

11

Chapter 3 Common Sampling Procedures

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By Common Carrier
Instructions

If the shipping container used is a picnic cooler, use tape to seal


the drain plug.

Nonhazardous
Samples

Hazardous
Samples

12

After acceptance by the shipper, tape the shipping container


completely around with strapping tape at two locations. Secure
the lid with tape. Do not cover any labels.

13

Place the laboratory address on the top of the shipping container.

14

For all hazardous shipments, complete shipper's hazardous


material certification form.

15

Place a This End Up label on the lid and on all four sides of the
shipping container.

10

11
Affix the signed and dated custody seals on the front right and
back left of the shipping container. Cover the seals with wide,
clear tape.
*Numbers indicate the instructions that must be followed.

Chapter 3 Common Sampling Procedures

16
17

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Table 3-2. Packaging Not by Common Carrier


Instructions
Quantity limitations shipped by cargo
aircraft
Gross weight of package:
Total quantity of flammable liquid:

Maximum sample container size:

Flammable
Liquid
66 pounds

DOT Class 9

Poison DOT
Class 6.1
66 pounds

66 pounds

Liquids
4 liters (1 gallon)
Solids
5 kilograms (11
pounds)

Liquids
4 liters (1 gallon)
Solids
5 kilograms (11
pounds)

49 CFR
172.101 Table,
Column 6b
49 CFR
172.101 Table,
Column 5 or
The flash point
of the liquid

Check the caps of all sample containers


to assure that they are secure. Tape
caps.

1*

1*

1*

Place each sample container in an


individual 6-mL plastic bag and secure
with a twist tie. The sample
identification tag should be positioned
to enable it to be read through the bag.

Place sample containers in paint cans in


a manner that will prevent bottle
breakage.

Place vermiculite in the paint can


around the samples. The amount of
vermiculite used should be sufficient to
absorb the sample if a sample container
should break.

Secure the lid to the paint can with can


clips and label the outside of the can
with the sample ID numbers and
quantity.

Wrap bubble wrap around each glass


sample container and fix with tape.
Package the paint cans in DOT boxes or
cooler. Use additional packaging to
secure cans.
Seal the drain plug with tape on the
inside and outside of the cooler and line
Chapter 3 Common Sampling Procedures

Liquids: 3

Solids: 4

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Instructions

Flammable
Liquid

Poison DOT
Class 6.1

DOT Class 9

Fill any voids in the cooler with


additional packing material.

Place ice contained in bags on top of all


sample containers within the cooler.
Use as much ice as space will allow.

Place the COC record in a clear plastic


resealable food bag and tape to the inside
of the cooler lid. Label the outside of the
cooler as containing the COC record.

the cooler with a plastic bag. Place the


canned or bagged sample containers in
the cooler. If plastic bottles are being
used, alternate them with any glass
container.

10
9
Seal the cooler lid with clear tape or
strapping tape. Affix security seals.
*Numbers indicate the instructions that must be followed.

Chapter 3 Common Sampling Procedures

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3.6.2. Marking and Labeling


All samples must be labeled to prevent misidentification and should include the following information:

Sample # or ID
Date of collection
Collector
Analysis requested
Preservative
Sample location.
Sample labels must clearly link the sample to the
field sheet or the COC record and must be written
legibly and in permanent ink. In addition, all
containers must be labeled and listed on the COC
record.
Note: If a three-bottle set is used for VOAs, all three bottles
must be labeled and listed on the COC record.

EPA TSCA regulations [40 CFR 761.40(e)]


require that a PCB label be put on all containers
whose surfaces are in direct contact with material
that is over 50 parts per million (ppm) PCBs.
This requirement applies to sample containers as
well as pails, drums, and other containers that are
in direct contact with the PCB material. The
labeling requirement does not apply to containers
in which PCB sample containers are shipped.
Although the sample containers must be individually labeled, this requirement is not affected by the
quantity of sample or whether the sample is classified as hazardous under RCRA or DOT regulations.
For DOT Class 9 and EPA Hazardous Waste the
following labeling requirements apply:

If EPA Hazardous Waste Manifest is


required:
- Hazardous waste
liquid, NOS, NA3082
solid, NOS, NA3077

If EPA Hazardous Waste Manifest is not


required:
- Environmentally hazardous substances
liquid, NOS, UN3082
solid, NOS, UN3077

Chapter 3 Common Sampling Procedures

OSHAs Hazard Communication Standard requires all containers of hazardous materials coming in or out of a workplace to be labeled with the
contents, appropriate hazard warnings, and the
name and address of the manufacturer. OSHA
does not specify a standard labeling method, but
some commonly used ones are provided by National Fire Protection Association (NFPA), Hazardous Materials Identification System (HMIS),
ANSI, and DOT.
3.6.3. Shipping Papers
Ship high hazard samples via overnight courier
following the couriers documentation requirements. A special airbill must be completed for
each shipment. An EPA manifest must be prepared if the shipping container contains hazardous waste unless the samples are exempt. The
Hazardous Waste Manifest must bear the
handwritten signatures of the generator, transporter, and designated facility. A copy of the manifest must be kept for 3 years by the shipper. The
shipping papers must contain the name, address,
and handwritten signature of the shipper.
The shipping papers (and Hazardous Waste Manifest if used) must contain a 24-hour emergency
response telephone number. This phone number
must be monitored at all times while the hazardous material is in transportation, including storage
incidental to transportation. The phone must be
monitored by a person who is either knowledgeable of the hazards and characteristics of the hazardous material being shipped and has comprehensive emergency response and incident mitigation information for that material, or who has
immediate access to a person who possesses such
knowledge and information. The emergency
response phone number must be entered on the
shipping paper immediately following the description of the hazardous material or entered
once on a shipping paper if the number applies to
all of the hazardous materials and is indicated for
emergency response information.
3.7. QA/QC Protocol
QC is a normal part of good field and laboratory
practice. QC includes all of the procedures apPage 3-23

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plied to data collection and generation activities


to achieve and maintain the level of preestablished data quality. The desired level of data
quality should be based on the intended use of the
data. Therefore, the QC protocol should include
all technical controls (e.g., sampling and analytical methods, use of field blanks, field duplicate
samples, inclusion of performance testing or
reference samples, statistical analysis, etc.). The
controls start with the regulatory requirements of
the data acquisition project and carry through to
the ultimate data reporting and completion of all
of the documentation of the use of these controls.
QA refers to the procedures used by management
to assure that the QC is what is required and that
it is being adhered to at any point in the project.
QA constitutes the overview and monitoring
processes designed to ensure that the quality of
the data generated meets the desired levels as
established by management. These controls
include establishing DQOs based on the intended
use of the data, the institution of procedures for
formalizing planning documents prior to the
initiation of data collection activities, and the use
of audits to identify problems in both QC and
QA.
The QA/QC protocol is specified in the SAP for
each job that involves field sampling. QA/QC
requirements are based on the level of data quality required for the project, and may address specific regulatory requirements. The purpose of a
QA/QC protocol is to ensure the following:

The laboratory receives samples that


accurately represent the conditions existing at
the sample site
The results of the analysis are traceable to the
specific sample location
Compliance requirements are met.
The methods used to attain this protocol include
training of personnel, providing detailed procedures for preparation, collection, marking and
handling, packaging, packing, transfer of samples, and validation and verification of the administrative process and sampling techniques.

Chapter 3 Common Sampling Procedures

3.7.1.

Decontamination of Sampling
Equipment
The SAP should address the extent of decontamination and specify the procedures to prevent
sample contamination. Sampling may be performed using separate laboratory cleaned equipment for each sample location. Procedure effectiveness should be checked for each matrix by
submitting equipment decontamination blank
samples to the laboratory for analysis.
Note: For specific information regarding the decontamination of field equipment, refer to ASTM D5088-02, Standard
Practices for Decontamination of Field Equipment Used at
Waste Sites. This standard describes the decontamination
process for field equipment used in the sampling of soils,
soil gas, sludges, surface water, and groundwater at waste
sites. According to this standard, these practices are applicable only at sites where chemical (organic and inorganic)
wastes are a concern, not for radiological, mixed (chemical
and radiological), or biohazard sites.

3.7.2.

Sample Container Cleanliness


Requirements
Sample containers are a possible source of sample
contamination. The SAP should specify the level
of QC for sample containers. Pre-cleaned containers meeting EPA CERCLA cleanliness endurance criteria are available from several suppliers.
If these containers are used, the serial number and
QA batch number of each one should be recorded
in the FLB/FN or on the field form. A review of
the cleanliness should be made to ensure all
parameters are checked to be below the detection
limit of the contaminants to be tested for compliance. Some SDWA and CWA parameters may
require laboratory cleaned containers proven to
be below the limit of detection for the method.
Note: In no case should an effort be made in the field to
decontaminate a sample container. If a container becomes
contaminated, it should be replaced, with a note to that
effect recorded in the FLB/FN.

3.7.3.

Sample Container Type and Size


Requirements
The types and sizes of sample containers to be
filled for each sample will depend on method
requirements and on QC requirements of the
SAP. General sample container requirements are
shown in Appendix B for different matrices and
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analytical parameters. Compliance with specific


instructions in the SAP is mandatory. If specified
sample containers are not available, permission
must be obtained from the Program Manager in
writing for the use of other sizes and types of
sample containers.

the field sampling or test plan must be followed


exactly. Any deviations from established test
procedures must be entered in the FLB/FN or on
the field form and the Program Manager must be
informed immediately of sample numbers affected.

3.7.4.

3.7.7. QC Samples
Field QC samples are prepared and analyzed to
determine whether test samples have become
accidentally contaminated, check on the repeatability of the method, and ensure the samples are
representative of the site or matrix sampled. A
number of different QC samples may be specified. Each of the QC samples checks for a potential problem that can affect data reliability. The
recommended frequency for each type of QC
sample is summarized in Appendix C.

Sample Preservation and Storage


Requirements
Special preservation and storage requirements
should be specified in the SAP to ensure that
samples do not undergo chemical changes from
the time they were collected until their analysis
by the laboratory. General requirements are
specified in Appendix B. The specific requirements of the SAP will govern.
The quality of the reagents, water and materials
used for preservation should be verified to ensure
these items do not invalidate the reported results.
Chemicals used as preservatives may be traced by
lot number and quality by maintaining a reagent
record keeping system. The water and acid preservatives used for trip and field blanks may be
checked prior to use in the field and lot controlled
to ensure no contamination is present prior to the
material leaving the laboratory.
3.7.5. Sample Holding Time Limits
Even with preservation and special storage procedures, the composition of samples can change
over time. The holding time for samples is the
time from collection to laboratory preparation or
analysis. Holding time limits summarized in
Appendix B are method and program requirements. Site-specific holding times specified in
the SAP take precedence.
3.7.6.

Laboratory and Field Analytical


Procedures
Laboratory analytical procedures for each parameter are specified based on the compliance
limits, permit limits and data needs stated in the
SAP. The SAP or COC record indicates to the
laboratory which sample containers are to be
analyzed for what parameters and specifies the
analytical methods. Based on the DQOs, field
testing may require the same level of QC as
laboratory testing, and the procedures specified in
Chapter 3 Common Sampling Procedures

3.7.7.1. Test Sample


The test sample consists of one or more sample
containers filled with material collected at one
sampling point within a stated time. Several
sampling containers may be required if material
collected for analysis for different parameters
must be preserved differently or sent to different
laboratories. For a specific test sample, all containers are designated by the same sample location number, but may have different sample
container numbers or designations to indicate
variations made to the samples.
3.7.7.2. Field Duplicates and Split Samples
Field duplicate samples are two separate samples
taken from the same source and are used to determine data repeatability based on field sampling
and laboratory analysis procedures. Field duplicate samples are as follows:

Assigned different container numbers


Specified in the FLB/FN or on the field form
Distinguished from the test samples on the
COC record or field records
Often submitted blind as to designation so the
laboratory data assures objectivity.
Exception: Each test sample collected for a specific organic analysis may consist of two or more containers filled
with the same material; these may be given different

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container numbers but are designated as the same sample


on the COC record. Only one sample container will be
analyzed; the other being saved as a backup in case the
laboratory must repeat the extraction and/or analysis.
Duplicate samples for analysis consist of sets of two containers, with each pair of containers being designated on the
COC record.

Field duplicate samples may be submitted to one


laboratory for analysis for the same parameters.
The comparability of the results provides information on the repeatability of the field sampling
and laboratory analysis procedures.
The containers may be submitted to different
laboratories for identical analyses to obtain information on inter-laboratory repeatability of
field sampling and laboratory analysis procedures. This is a split sample.
Sample heterogeneity may cause major problems
with the representativeness of field duplicate or
split samples of soil/sediment matrices. Proper
sample homogenization in the field will significantly improve the repeatability of the field sampling procedure. (Gy P. 1993, Sampling for
Analytical Purposes, Wiley, West Sussex. Pitard
F. F. 1993, Pierre Gys Sampling Theory and
Sampling Practice: Heterogeneity, Sample Correctness and Statistical Process Control, Books
Britain, London.)
Typically, both field duplicates and split samples
will be collected at a rate of 10% of field samples
or at a minimum of one, per analyte, matrix, and
sampling technique. More duplicates and split
samples may be collected depending on the data
quality needs.
3.7.7.3. Equipment Decontamination Blanks
Equipment decontamination blanks, or rinsate
blanks, provide information on the levels of
cross-contamination resulting from field or laboratory sample preparation actions. These blanks
are specified in the SAP and on field sampling
forms, and are prepared in the field. An equipment decontamination blank is usually reagent or
deionized water that is free of the analyte of
interest and is transported to the site, opened in
the field, and poured over or through the sample
collection device, collected in a sample container,
Chapter 3 Common Sampling Procedures

and returned to the laboratory and analyzed. This


serves as a check on sampling device cleanliness.
For example:

Field Groundwater Equipment Decontamination Blank for Metals Analysis. Handled


by the bailer, use ASTM Type II water, or
better. Filter, place in a sample container, and
preserve using the same procedures as for the
test and duplicate samples.
Soil Sampling Equipment Decontamination
Blank for Semivolatile Organics. Rinse the
field equipment prior to its use and collect the
rinsate for analysis.
PCB Wipe Sample Equipment Decontamination Blank. Use a wipe pad to wipe the
sampling template in the same way the pad is
handled during the actual wipe sampling of a
surface.
One equipment decontamination blank is collected for each type of equipment used during the
day or sampling event. Equipment decontamination blanks are assigned container numbers from
the same sequence as the test samples, and may
not be distinguished from the test samples on the
COC record. More blanks may be collected
depending on the data quality needs.
3.7.7.4. Field Blanks
Field blanks are prepared and analyzed to check
cleanliness of sample containers, environmental
contamination, and purity of reagents or solvents
used in the field. A sample container is filled
with laboratory ASTM Type I or II water, preserved, shipped to the field with clean sample
containers, opened in the field to exposure to
ambient field air for a time compatible to field
sampling process, and is closed and submitted for
analysis using the same parameters as the test
sample. The reported results will indicate the
presence of contamination. Field blanks are most
often used when measuring for volatile analytes.
3.7.7.5. Trip Blanks
A trip blank is used with VOA analysis of water.
A blank may consist of two 40-milliliter VOA
vials filled at the laboratory with laboratory
ASTM Type I or II water, transported to the
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sampling site and returned to the laboratory without being opened. This serves as a check on
sample contamination during sample transport
and shipping.
Note: The caps used on VOA vials have Teflon-lined
septa. The Teflon side of the silicone septum should face
the sample. Prior to closing a vial, make sure there is no
soil particle or dirt on the sealing surface of the VOA vial to
prevent leaks. If a high concentration of volatile chemicals
is present in the air in a shipping container, these chemicals
can pass through the septum and contaminate the sample.

A trip blank is included in each shipping container used to ship VOA water samples. One VOA
trip blank (two vials) is submitted to the laboratory in each cooler or per sampling event. The
frequency of collection for trip blanks is specified
in the SAP and is based on the data quality needs.
Trip blanks are assigned container numbers from
the same sequence used for the test samples, and
are not designated as blanks on the COC record.
3.7.7.6. Matrix Spike (MS)/Matrix Spike
Duplicate (MSD)
Project or compliance QC procedures require that
the laboratory spike a portion of the matrix with a
predetermined quantity of analyte(s) prior to
sample extraction/digestion and analysis. The
frequency of performing an MS is dependent on
the data quality needs and method requirements.
A spiked sample is processed and analyzed in the
same manner as the sample. The result of the
analysis of the spike compared with the non-spike
sample indicates the ability of the test procedures
to recover the analyte from the matrix, and provides a measure of the performance of the analytical method executed by the laboratory.
For an MSD, a second portion of the matrix is
spiked, and the recovery of the MSD can be
compared with the recovery of the MS.
Depending on the matrix and analysis, additional
sample containers may be specified to provide
enough material for this laboratory procedure.
These sample containers are assigned container
numbers from the same sequence as the test
samples and are designated MS/MSD materials
on the COC record.

Chapter 3 Common Sampling Procedures

The MS/MSD samples are commonly used in


CERCLA testing, but are not commonly used in
CWA or SDWA testing. MSs are routinely performed by the laboratory as part of its internal QC
on randomly chosen samples. If MS data is
required for SDWA or CWA reporting requirements, a request must be made to the laboratory
to ensure the MS is performed and reported on
the appropriate sample. The sample selected for
MSs should have the same or similar matrix as
the field samples but without high levels of
target analytes.
3.7.8. Field Audits
The SAP will specify who will conduct field
audits, along with their frequency and procedures.
QA/QC procedures of the sample collection effort
must identify and determine the magnitude of
error associated with the contamination introduced through the sample collection effort.
Audits are perhaps the most effective tool to
ensure that the sampling is done correctly. The
two factors most likely to influence the magnitude of the sample collection error are collection
methods and frequency of sampling.
In general, a field sampling audit provides an
independent outside check on the following:

Field Records
- COC records
- Sample container labels
- FLBs or field forms
- Personnel training records
Sampling Procedures
- Equipment
- Sample containers
- Accuracy of sample location
descriptions
- Comparability of field sampling
techniques
- Collection and preparation of QC
samples
- Sample preservation
- Equipment decontamination
- Contaminated waste storage and
disposal

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- Sample packing, storage, security, and


transportation
- Shipping containers, including use of
custody seals (if applicable).
3.8. Generic Sampling Equipment List
Equipment specific to each type of media is
found at the end of the related chapters. The
following is a generic sampling equipment list:

Map of sampling location(s)


Sampling SOP
FLB or field form
Pens
Containers
Preservatives
Labels

Chapter 3 Common Sampling Procedures

Markers
Coolers
Ice
Packing material
Packaging tape
COC form
Custody seals (if required)
Decontamination storage containers,
equipment, and materials
Personal safety equipment, safety test
equipment
Field screening or testing equipment,
standards, reagents, and SOP
Testing field forms or logbooks
Laboratory instructions (if different from
custody form).

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Chapter 4. Soil Sampling


4.1. Purpose
This chapter identifies the major steps that are
required and technical areas that will be encountered when soil sampling. The scope of the sampling program is defined, as well as procedures
that will guide the sampler in conducting soil
sampling.
4.2. Scope
The characterization of soil and soil contamination requires a collection of samples from identifiable locations. Soil sampling programs can
accomplish the following:

Determine site soil characteristics (presence


and location of different types of soil, subsoil,
and bedrock)
Define the extent, depth, type, and severity of
soil contamination
Determine soil cleanliness during procedures
such as UST removal, or PCB transformer
operation
Soil sampling programs also can provide for
background monitoring at treatment, storage,
and disposal facility (TSDF) or hazardous
waste handling areas.
4.3. Project Planning
This section provides an overview of the planning
process for conducting soil sampling. Included is
a discussion of sampling strategy, development of
a site-specific SAP, and QA considerations.
Before soil sampling can begin, clear and concise
objectives regarding the intent of the sampling
program need to be developed. The objectives
provide the framework for developing a sampling
strategy for the site and preparing the SAP. Once
the objectives are established, a sampling strategy
can be developed.
4.3.1. Sampling Strategy
The sampling strategy is designed around the
objectives of the project and should begin with a
review of the conceptual site model. The model
Chapter 4 Soil Sampling

takes into consideration historical site use, known


or suspected pollutant releases, and the geology
of the area. The conceptual site model is dynamic and is constantly revised as new information is
collected and processed. The model focuses on
contaminant fate and transport processes, the
control of geologic materials on the contaminant
pathways (e.g., depositional environments, geologic structure), the types of contaminants present
(e.g., hydrophobic versus hydrophilic), and the
processes that influence the concentrations of
contaminants present (e.g., dilution, biodegradation, dispersion).
The detail of the conceptual site model will depend greatly on the availability of information
including historical site uses, native soil type,
areas where fill materials may be present (e.g.,
utility trenches), and the direction of surface
water flow. Specifically, the conceptual site
model should describe:

Physical characteristics of the site, including


locations of buildings, paved areas, subsurface
utilities, overhead utilities, significant
topographical changes (e.g., steep banks),
exposed bedrock, standing water, stained soils,
areas of depressed vegetation, equipment
maintenance and storage areas, manufacturing
locations, waste disposal areas, and expected
depth to groundwater
Types of contaminants to be sampled (e.g.,
volatile organic chemicals (VOCs), semiVOCs, metals) and factors that could bias
sampling results (e.g., organic contaminants
that are tightly bound to soil particles)
Lateral and vertical distribution of
contamination (e.g., contaminants distributed
throughout an entire unit being monitored
versus localized distribution controlled by
small-scale features).
The sampling strategy and the information gathered from the conceptual site model will become the framework for development of the sitespecific SAP. Key issues related to the concepPage 4-1

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tual site model are presented in more detail in the


following subsections.
4.3.1.1. Types of Contaminants
The sampler or Site Manager may be able to
predict the types of soil contaminants present and
the duration of contamination by consulting site
historical records and information on previous
manufacturing practices, fuel or chemical usage,
and any reported spills. This information can be
used to determine sample collection locations.
For instance, heavy metals such as oxidized lead
or organic chemicals such as pesticides which are
relatively insoluble in water may be limited to the
top few inches of soil and will not have spread far
from their source in undisturbed sites. However,
if sites are affected by soil erosion or construction
activities, the contaminants may have moved
from their source, and sampling program planners
should account for these changes in site conditions. The extent to which the underlying
groundwater is contaminated also would be a
function of the solubility of the organic liquid in
the water. Dense non-aqueous liquids, such as
chlorinated solvents (e.g., trichloroethylene,
tetrachloroethylene, carbon tetrachloride) or
heavier chlorinated organic liquids (e.g., chlorinated benzenes, PCBs), can permeate the subsurface until they reach a confining layer, such as
clay or bedrock.
For soil contaminants such as soluble metals
found in metal plating wastes or from spills of
concentrated organic chemicals (e.g., gasoline,
aviation fuel, solvents, and transformer oil), the
presence and extent of contamination may not be
easily predictable due to a number of factors.
Soluble metals and organic liquids often are
carried through soil by percolating rain water.
The extent of contaminant movement is affected
by a number of factors, including:

Density of Organic Liquids. Light organic


liquids (e.g., gasoline, diesel fuel, and waste
oils) will settle through soils that are not
saturated with water until they reach a
confining surface such as clay, bedrock, or
groundwater. It is not unusual to find a

Chapter 4 Soil Sampling

concentrated layer of organic liquid moving


along the surface of a tilted clay layer or
forming a pool or lens on the groundwater.
Therefore, the extent to which the underlying
groundwater is contaminated, is a function of
the solubility of the organic liquid in the water.
Dense, non-aqueous liquids, such as
chlorinated solvents (e.g., trichloroethylene,
tetrachloroethylene, carbon tetrachloride) or
heavier chlorinated organic liquids (e.g.,
chlorinated benzenes, PCBs) can continue to
sink through groundwater until they reach a
confining layer, such as clay or bedrock.
These chemicals can flow along tilted surfaces
or pool in the cracks in bedrock and then
slowly leach into groundwater.
Susceptibility to Biodegradation.
Microorganisms in the soil can degrade many
contaminants. However, for contaminants like
fuels or other petroleum distillate products, the
microorganisms require oxygen and generally
are not active at depths of more than 1 foot.
Therefore, the surface soils may be relatively
uncontaminated by these organic chemicals
due to biodegradation, while deeper soils may
be contaminated due to the lack of oxygen
needed for biodegradation.
4.3.1.2. Type of Soil
Soil type can have a significant impact on the
mobility of pollutants. For example, clay layers
create relatively impermeable barriers, retarding
groundwater flow and in some instances preventing surface contaminants from affecting groundwater. However, clay particles also can absorb
certain types of hazardous chemicals, resulting in
increased pollutant concentrations in localized
areas. Organic liquids can form pools in the low
reaches of clay layers, or can flow down the
surface of tilted clay layers.
Soils that contain large amounts of organic material, such as peat, can absorb and concentrate
hazardous chemicals. A layer of organic soil,
therefore, may be more contaminated than the
soil layers above and below it.

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Porous non-organic soils, such as sand or gravel,


do not absorb pollutants and allow for rapid
surface and groundwater movement. In such
soils, PCBs from spilled transformer fluid and
from buried electrical capacitors have been found
several hundred feet from the source of the contamination. Gasoline from leaking USTs can be
carried hundreds of feet by moving groundwater.
Bedrock may provide a confining layer beneath
groundwater. Fractured bedrock, however, may
provide channels for the movement of groundwater and heavy organics or low spots for the accumulation of pools of heavy organic liquids.
Soil characteristics such as pH, can change the
chemistry of the surrounding water, which in turn
can affect the solubility of some pollutants, including heavy metals. For instance, acidic
stormwater can dissolve metals on the ground
surface. However, as the dissolved metals pass
through the soil column, they may encounter
areas with elevated soil pH (e.g., limestone) that
cause the metals to become insoluble precipitates
again.
4.3.1.3. Presence of Groundwater
Moving groundwater can carry hazardous contaminants for considerable distances; see Figure 41.
Figure 4-1. Contaminated Groundwater

The rate at which groundwater will cause contaminants to spread is affected by both the speed at
which the groundwater moves through the soil
Chapter 4 Soil Sampling

and the extent to which the soil absorbs the contaminants. One of the most serious effects of
accidental spills and improper disposal of hazardous chemicals is contamination that precludes the
use of a groundwater source for drinking water.
4.3.2. Site-Specific SAP
A soil sampling program should collect soil
samples at a specific locations and depths that are
representative of the site. Procedures that result
in the collection of an undisturbed soil column
will yield the most representative soil samples.
The development of a site-specific SAP is the
first step toward collecting a representative soil
sample (see Chapter 2 for a detailed discussion of
SAP development applicable to all sampling
programs). Each SAP is an instruction manual
for field personnel, and should be built around the
objectives and sampling strategy. The discussion
below focuses specifically on SAP development
for soil sampling programs.
Ideally, the SAP should be based on knowledge
of which contaminants are likely to be present
and how the distribution of the contaminants may
be affected by the soil characteristics of the site.
The purpose of the fieldwork also may be to
define the soil characteristics and obtain chemical
data for determining compliance with federal,
state, or local requirements. It is possible for soil
sampling to be conducted in a number of phases,
with the field observations and field test results
providing data to guide subsequent work. If
knowledge of contaminants and site soil characteristics is limited, then dynamic sampling techniques and field measurements can be used to
locate sampling points.
Dynamic sampling relies on individuals in the
field to interpret field data as it becomes available
and revise the sampling strategy accordingly.
Dynamic sampling can quickly provide significant amounts of information needed to develop
the conceptual model for the site. Dynamic
sampling in many instances, however, is considered a first step toward developing a more focused soil sampling program for a particular area
within the site.
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The SAP should consider a variety of factors,


including, but not limited to, the physical features
of the site (e.g., locations of buildings, tanks,
buried utilities, roadways), the types of contaminants and their potential mobility and biodegradability, soil types, the accessibility of potential
sampling locations, the size of equipment needed
to collect samples at depth, suspected pollutants,
field screening requirements, DQOs, analytical
methods and detection limits, soil collection
methods, sample handling procedures (e.g., preservation requirements, COC), containment and
disposal procedures for contaminated soils generated during sampling activities, and safety.
The SAP cannot be implemented effectively if
field personnel do not understand its contents.
Many times the primary reason that sampling
events are problematic is that the person who
prepared the SAP is not the person in the field.
One method that alleviates this problem is assigning a Sampling Team Leader who is responsible
for all activities in the field. The Sampling Team
Leader will work closely with those individuals
preparing the SAP to understand fully the objectives of the program. The Sampling Team Leader
then will be responsible for all individuals in the
field. He or she also is responsible for providing
additional training to field personnel, if required,
before fieldwork begins.
4.3.3. QA
Soil sampling programs encompass a variety of
information sources and include both primary and
secondary data collection. These data sources are
used to continuously update the conceptual site
model and allow site managers to make decisions
regarding further investigation, additional monitoring, remediation alternatives, or site closure.
The level of data quality for each soil sampling
program, and for each specific sampling event,
depends on the intended use of the data. For
example, the level of QA/QC needed to estimate
the volume of soil that may need to be removed
for a corrective action might be different than for
samples needed for site closure. It is important to
remember, regardless of the level of QA/QC for
Chapter 4 Soil Sampling

any soil sampling event, that sample integrity


must be maintained during sample collection.
Laboratory analysis, no matter how sophisticated,
is defensible only if the sample supplied to the
analyst has retained its integrity.
To ensure quality data, site managers and those
responsible for data integrity should begin with a
systematic planning process that helps define the
DQOs. The DQOs clarify the study objective,
define the most appropriate type of data to collect, determine the most appropriate conditions
for data collection, and specify tolerable error
limits that will be used as the basis for program
decision making. Detailed information on
QA/QC, including the systematic planning
process, development of DQOs, and preparation
of SAPs, is available in Chapter 2 of this handbook.
Some specific QA/QC issues related to soil sampling programs include equipment specifications,
equipment decontamination, and QC samples.
Each of these is discussed briefly in the following
sections.
4.3.3.1. Secondary Data
Secondary data are those data collected in addition to sampling data. For a soil sampling program, secondary data may include items such as
historical records regarding site use, spills, and
corrective actions on neighboring properties,
current and historical subsurface utility maps,
locations of previous above-ground and belowground structures as well as possible disposal
areas and areas containing fill materials or other
antidotal agents. These data aid the Site Manager
in selecting soil sampling locations or determining possible pollutants.
For secondary data, acceptance criteria are used
instead of the measurement performance criteria
typically used for laboratory data. In general,
acceptance criteria are used to assess secondary
data adequacy and evaluate uncertainty in the
results derived from the use of secondary data
sources. For example, the Project Manager for
the soil sampling program may require interviews
of former employees to validate the location of
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disposal areas found on historical site maps. In


this case, the acceptance criteria are the verbal
confirmation of the disposal areas by the former
employees. The SAP for each soil sampling
program will explain the acceptance criteria for
determining which sources of data are sufficient
to support the project objectives. See Chapter 2
for more information.
4.3.3.2. Equipment Specifications for Quality
Control
The selection of appropriate materials for soil
sampling equipment is critical to ensuring data
quality. The materials that come into contact
with the sample are as critical as the composition
of the laboratory sample containers. Selecting the
appropriate materials for sampling equipment
should be based on the type of expected pollutants. It is important that the sample equipment
not add or remove target pollutants. For example,
if collecting samples for analysis of low-level
metals, carbon steel sampling equipment should
not be used. If samples are being collected for
low-level organic constituents, plastic sampling
equipment should be avoided because plastics
have the potential to absorb organic pollutants.
The recommended materials for hand augers, split
spoons, trowels, and other sampling devices are
as follows: polytetrafluoroethylene (PTFE) (Teflon), stainless steel, polypropylene, linear polyethylene, polyvinyl chloride (PVC), Viton,
and conventional polyethylene. Because soil
sampling typically requires more rugged equipment compared with other types of sampling,
stainless steel equipment is typically the material
of choice.
4.3.3.3. Equipment Decontamination
Decontamination of existing and new equipment
is required prior to use in the field. Section 4.9
describes decontamination procedures for various
types of soil sampling equipment. Decontamination procedures must be followed and documented to prevent cross-contamination between
sites and within the site. Rinsate blanks may be
collected at the start and end of the sampling
event to determine the cleanliness of the sampling
Chapter 4 Soil Sampling

devices and evaluate the cleaning techniques used


in the field. Decontamination procedures for all
equipment that contacts soils must be included in
the SAP.
4.3.3.4. Quality Control Samples
Field duplicates or splits are collected in the field
in double the number of bottles required for the
regular sample. A duplicate sample is a sample
collected concurrently, under comparable conditions, with a first sample. Duplicate samples are
QC samples that are used to assess data repeatability based on field conditions. Duplicate samples provide a total precision of field sampling
precision and lab analysis. Duplicate samples
should not be identified as duplicates to the laboratory. Split samples are two or more representative portions taken from one sample in the
field or in the laboratory and analyzed by different laboratories. Split samples are QC samples
that are used to assess analytical variability and
comparability. Samples sent to the same laboratory are duplicates, and samples sent to a different
laboratory are splits. Split samples shall be field
homogenized. To ensure that split samples are
representative, the soil sample collection must
follow Pierre Gys Sampling Theory and Sampling Practices. However, for VOC samples,
split samples shall be collected as field duplicates
to minimize loss of volatile components.
Procedures for obtaining split soil samples are
included in Section 4.7.4.3.
4.4. Hazards and Safety Precautions
The HASP should address all anticipated hazards
for each task. The following discussion contains
common (and commonly overlooked) hazards
associated with soil sampling activities. Refer to
Chapter 2 for references to specific hazard identification techniques and detailed control measures.
4.4.1. General Safety
Some of the general safety hazards associated
with soil sampling programs include the following:

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Moving sampling equipment and containers


across rough terrain either by hand or by
driving off road
Use of heavy equipment such as drill rigs and
power augers
Conflicts with other uses of the area (e.g.,
traffic conflicts when sampling on or next to
roads)
Contact with overhead power lines when using
a drill rig or a backhoe to gain access to
subsurface soil.

4.4.2.3. Toxic Chemicals


Collecting soil samples poses the risk of exposure
to hazardous chemicals. The following major
exposure scenarios should be evaluated:

4.4.2. Subsurface Hazards


Soil sampling is an intrusive activity that could
expose sampling personnel to unidentified subsurface hazards, as discussed below.

4.4.2.1. Buried Munitions


If the probability of encountering buried munitions during the sampling program is moderate to
high, a Required Explosives Safety Submission
(RESS) waiver from the relevant explosives
safety authority may be required prior to disturbing the site. In addition, a qualified explosives
safety expert will be required to accompany the
investigation team. See DoD TP18 for the minimum qualifications for unexploded ordnance
technicians and personnel. The site should be
checked by qualified personnel with groundpenetrating radar and/or metal detectors before
any samples are collected. Only trained and
certified personnel should handle or sample
explosive or suspected explosive materials.
4.4.2.2. Buried Utilities
The use of augers and drill rigs to gain access to
subsurface soil can damage buried utilities, including electrical and telephone lines and gas,
steam, water, and industrial pipelines. Facility
records should be reviewed carefully to identify
any buried utilities in the sampling area. The site
should be checked with ground-penetrating radar
and/or metal detectors if there is any question as
to the presence of subsurface utilities.

Chapter 4 Soil Sampling

Skin Contact with Contaminated Soil. Field


sampling personnel should wear disposable
boot covers and surgical gloves as a minimum,
and should consider the use of disposable
Tyvek coveralls to prevent contamination of
clothing. The sample custodian should wear
appropriate PPE when handling samples.
Skin Contact with Contaminated Water.
Deep soil samples usually result in the
requirement to handle wet soil that can drip
and splash. Decontamination of sampling
equipment also can result in splashes of
contaminated water. Field sampling and
decontamination personnel should wear
waterproof rain gear or coated Tyvek
coveralls if there is a possibility of contact
with contaminated water.
Ingestion of Contaminated Soil. Ingestion
can occur when food or drink is exposed to
contaminated dust or is picked up with
contaminated gloves. Field personnel should
not eat, smoke, or chew gum or tobacco when
working with contaminated soil. Drinking
water should be kept in closed squirt bottles or
should be stored outside the contaminated
area.
Inhalation of Contaminated Dust. Inhalation
of contaminated dust may be a problem on dry
windy days at sites where the surface soil is
contaminated. Digging and drilling activities
also may generate contaminated dust.
Personnel should remain upwind of any source
of dust. If the site is generally contaminated,
then full-face, air-purifying respirators
equipped with particulate filters should be
worn.
Inhalation of Toxic Vapors. The exposure of
contaminated soil to ambient air may generate
toxic vapors from the evaporation of VOCs.
The HASP should establish air monitoring
requirements for intrusive work and specify
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the type of air monitoring equipment to be


used as well as the criteria for the use of
respirators. Either air-purifying respirators or
supplied-air respirators may be required,
depending on the toxicity of the chemicals
present, the capabilities of the monitoring
equipment, and the warning properties of the
vapors.
Confined Space Hazards. In general, pits
more than 4 feet deep are considered to be
confined spaces. However, any pit dug in
contaminated soil could have the same hazards
associated with confined spaces because
flammable vapors or toxic gases, including
hydrogen cyanide and hydrogen sulfide, could
accumulate. All applicable confined space
entry requirements should be imposed and
detailed in the HASP.

considerations are required when sampling explosive wastes that are susceptible to shock, friction,
electromagnetic radiation, electrostatic discharge,
sparks, flames, elevated or freezing temperatures,
moisture, or sunlight. Failure to handle explosives correctly could result in damage to property,
injury, or loss of life. For explosives safety and
handling requirements, refer to DoD 6055.09-M,
DoD Ammunition and Explosives Safety Standards. For Navy projects, also refer to NAVSEA
OP5, Volume 1, Ammunition and Explosives,
Ashore Safety Regulations for Handling, Storing,
Production, Renovation, and Shipping.

1. Ventilate the area thoroughly prior to entry.

General explosives safety considerations include


wearing PPE such as flameproof clothing, caps,
safety goggles or face shields, conductive shoes,
and respirators, where appropriate. Only nonsparking tools should be used. Electrical grounding may be necessary in some cases. Sampling
of the smallest amount necessary to perform
testing is recommended. Specific precautions are
material-dependent. It is imperative that sampling
personnel have a thorough knowledge of the characteristic dangers and safety requirements for
individual explosives materials.

2. Disconnect connecting pipelines.

4.5. Principles of Sample Collection

3. Take air samples to verify the absence of


flammable or other hazardous vapors and
demonstrate the presence of adequate oxygen
levels.

The collection of quality soil sampling data requires documentation of site surface conditions
(e.g., locations of buildings, pavement, standing
water, seeps, sediment runoff, discolored soil)
and subsurface conditions such as depth of various layers of soil, depth to groundwater and
bedrock at different locations. The chemical data
obtained from the analysis of soil samples is
useful only within the context of these site conditions, so it is imperative that the exact location of
each sample be documented and the soil samples
accurately represent the conditions at the site.

WARNING: Personnel who enter into a confined space


should be accompanied by an on-site standby unit at all
times.

The following steps should be detailed in the


HASP prior to entry into a confined space:

4. Provide entry and standby teams with proper


training, respiratory protection, protective
clothing, safety harnesses, and ropes.
5. Establish lifeline signals (e.g., tugging on a
rope) prior to entry so that Field Sampling
Personnel can communicate.
6. Maintain ladder(s) and other equipment in
accordance with OSHA regulations.
4.4.3. Explosive Hazards
Due to the inherent dangers involved in sampling
explosives and potential or suspected explosives,
only those individuals who have been trained and
certified in the proper handling of these materials
should participate in sampling activities. Special
Chapter 4 Soil Sampling

Soil samples must represent field conditions and


address the data needs of the program. For instance:

In determining whether the contamination of


surface soil presents a hazard by skin contact
or ingestion, the samples should consist of soil
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from the surface to a depth of only 2 inches,


and the soil should be sieved to eliminate
stones larger than 2 mm in diameter.
EPA cleanup requirements for soil
contaminated with PCBs are based on the
concentration of PCBs in the soil, including
rocks. The samples taken to define the
location of PCB-contaminated soil and the
appropriate remediation criteria should not
eliminate rocks, because the cleanup standards
are based on the maximum allowable average
concentration of PCBs in the remaining soil.
To determine whether excavated soil is
classified as a hazardous material under
RCRA, soil samples should be representative
and include rocks and hard chunks. The
extraction procedure specified by EPA may
require that the lab screen the soil to eliminate
rocks larger than 3/8 inch in diameter, but the
criteria are too complicated to allow a decision
to be made in the field as to whether the soil
should be screened when it is collected.
Special sampling procedures must be used
when collecting soil samples that will be
analyzed for VOCs because these chemicals
rapidly evaporate from soil once exposed to
the air. Unless precautions are taken to
minimize this evaporation, the samples will
not be representative of the actual level of
contamination of the soil.
Another important data requirement from any
field sample is the documentation of the exact
location where the sample was collected. Stakes
or flags should be installed to indicate the locations of soil samples. However, because sites
probably will be disturbed by subsequent construction work, it also is important that the location of each sample be measured with reference
to permanent features such as survey monuments,
measurements to a reference point, or latitude and
longitude location. For soil sampling programs, it
is generally acceptable for the survey to define
each sample location to an accuracy of 1 foot
horizontally and a few inches vertically. Unless
the area to be sampled is flat, an initial survey
should be made to define the surface contour.
Chapter 4 Soil Sampling

Measuring the depth from the surface at which a


sample is taken and at which different soil layers
and groundwater are encountered is insufficient,
unless the elevation of the surface at that point is
known and will remain undisturbed.
The final important data requirement is the physical characteristics of the site, including the surface
soils, subsurface geology and soil characteristics.
The physical characteristics of surface soils help
define the initial locations for soil borings and aid
in selecting the appropriate laboratory analyses for
future soil samples. The following locations and
physical characteristics should be noted and included on a site map:

Erosion patterns and accumulated runoff


sediments
Equipment or activities, including aboveground and underground storage tanks,
chemical storage buildings, outdoor areas
where servicing of automotive or mechanical
equipment has occurred, raw material storage
areas, locations of lagoons, waste pits and fire
pits, and locations where trash is either
disposed or stored temporarily, such as in
dumpster areas
Discolored soil
Areas covered by impermeable material, such
as pavement and buildings
Areas of distressed vegetation
Exposed bedrock
Standing water
Groundwater seeps.
Subsurface geology and soil characteristics are
typically determined during the site investigation
phase of a soil sampling program and are used to
predict pollutant movement and develop alternatives for any potential remedial actions that may
be required. Subsurface geology and soil characteristics data include the following:

Type of soil as a function of depth at each


sample location (e.g., layers of clay, peat,
sand, silt, shale, layers having different colors
or the presence of large stones)
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Soil moisture at different depths, and the depth


at which the soil becomes saturated with water
(i.e., depth to groundwater)
Presence of organic vapors in soils at various
depths.
Field sampling personnel often are in the best
position to detect areas of suspicion and, therefore, are critical to the success of the sampling
program. Though sampling techniques may be
sophisticated, they should not be relied upon to
replace the good judgment and common sense of
sampling personnel in discerning the difference
between routine and extreme case scenarios.
Sampling personnel must be alert to their surroundings (e.g., unusual circumstances, odors,
presence of dead animal or plant life in the area)
while conducting the following sampling tasks:

Collecting and recording visual and physical


data
Collecting soil samples, both surface and
subsurface
Adhering to field sampling and safety
procedures
Maintaining the COC record
Preserving program integrity.
Techniques for preparing a site map and documenting field data and observations are discussed
below.
4.5.1. Preparation of Site Map
Documentation of site conditions and sample
locations requires a site map. The site map
should be included with the SAP. The site map
may be based on facility drawings but should be
verified in the field and augmented with additional information on the drainage of rainwater and
other surface conditions that affect the movement
of contaminated soil. If the SAP does not include
a site map, one should be prepared by Field Sampling Personnel based on the availability of facility drawings and field measurements.
Integrating a geographic information system
(GIS) into a sampling program allows for creating
maps in significantly less time compared with
Chapter 4 Soil Sampling

traditional computer aided design (CAD) procedures. GIS-based data analysis is quicker, easier,
and more accurate compared with traditional
CAD methods. GIS can be used to analyze site
conditions such as depth to groundwater, saturated thickness, hydraulic conductivity, and soil
type for selection of suitable sampling points as
well as for analyzing relationships between sample locations, tracking sampling points, and relocating sampling points under changing site conditions.
The basic tools necessary for incorporating a GIS
into a sampling program include a global positioning system (GPS) unit/receiver and a computer program such as the ESRIs ArcGIS. The GPS
receiver is used to locate predetermined sampling
points in the field and/or record the location of
sampling points as samples are collected. The
GIS program can be used to analyze site conditions prior to the sampling event or map and
analyze the collected data. Creating a GIS database at the early stages of the sampling process
provides for an effective method for data management, analysis, and presentation. The use of a
GIS can significantly streamline many aspects of
a soil sampling program and facilitate the exchange of resultant data among stakeholders.
Site maps, whether prepared using GIS- or CADbased systems, should include surface contour,
surface information, and sampling locations, as
discussed below.
4.5.1.1. Surface Contour
Unless the site is completely flat, it is important
that the surface contour be indicated on the site
map. The depth of soil samples is measured from
the surface, but the surface reference can be lost
due to excavation or filling activities at the site.
If a contour map of the site is not available, it
may be necessary to have one prepared by a
survey team prior to sampling.
4.5.1.2. Surface Information
Sampling personnel should validate the site map
before beginning any sampling activities, noting

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any discrepancies. The following surface information should be recorded if not already shown:

VOCs in soil vapor. Each of these preliminary


tests and observations is described below.

4.5.2.1. Weather Conditions


The weather conditions at the time of sample
collection should be noted in the FLB/FN.
Weather data should include temperature, relative
wind speed and direction, relative humidity, and
the presence of rain or snow. Recent weather
conditions at the site should be summarized,
including recent rain events (how much and how
recently) and freezing conditions (how cold and
how deeply is the soil frozen).

Buildings or structures
Paved areas
Unpaved roads and parking areas
Surface areas with different types of soils,
including fill areas (e.g., gravel roads, clay,
sand, peat)
Standing water, both permanent (e.g., ponds
and streams) and temporary (e.g., persistent
puddles)
Water seeps
Water runoff patterns and accumulations of
runoff sediments
Exposed bedrock
Discolored soil
Stored materials, debris, and soil piles
Vegetation, including distressed vegetation.
Photographs should be taken to document site
surface features. Photography requirements
should be established by the Program Manager to
ensure compliance with the policy and regulations of the facility.
4.5.1.3. Documentation of Sampling
Locations
The location of each sample and the designated
sample numbers should be shown on the site
map. Samples should be collected at the designated sampling points. Depth of samples from
the surface should be recorded. If it becomes
necessary to sample more than 1 foot from the
required location due to interferences from trees,
pavement, subsurface rocks, or buried utilities,
the new sample location should be noted on the
map, and the reason for moving the sampling
location should be explained in the FLB/FN.
4.5.2. Preliminary Tests and Observations
A number of field tests and observations may be
required to document sampling and subsurface
conditions. Such tests may include weather
conditions at the time of sampling, a description
of the subsurface geology, and the presence of
Chapter 4 Soil Sampling

4.5.2.2. Description of Soil Types and Soil


Characteristics
The movement of groundwater and the transport
of hazardous chemicals are strongly influenced
by the presence and depths of different types of
soil. Knowledge of subsurface soil characteristics
is necessary to understand the dynamics of soil
contamination.
The soil should be described by a professional
geologist if this information will be used to support the computer modeling of groundwater
flow. If this level of detail is not required, the
soil layers and the soil samples should be described by Sampling Personnel.
Chapter 3 of EPAs Description and Sampling of
Contaminated Soils A Field Pocket Guide is a
good source for the field description of soils. As
necessary, the following soil features should be
described as a function of the depth from the
surface:

Color. Soil colors should be determined with


the use of a color chart, such as a Munsell
chart
Mottles. Blotches or spots of contrasting color
interspersed with the dominant soil color
Soil Texture. This is the amount of sand, silts,
and clays in a soil
Particle Shape. Shape of individual soil
particles
Structure. Shape of the natural soil
aggregates
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Consistency. Degree of resistance to breaking


or crushing (descriptions will vary with
moisture condition)
Presence of Visible Organic Liquids. Such
as oil, gasoline, solvents or other
Horizon Thickness. Layers of soil with
distinct changes of the above features.
4.5.2.3. Soil Gas
Soil gas monitoring is primarily used to measure
characteristics of the soil atmosphere as an indirect indicator of VOC contamination in soil or
groundwater. The resulting information may be
used to:

Detect and monitor migration of volatile


contamination of soils within the vadose zone
Support the design of a soil vapor extraction
system
Assess the extent of groundwater volatile
organics contamination
Verify UST integrity
Monitor for any subsurface discharges
Target soil borings
Aid in placing groundwater monitoring wells,
extraction wells, or recovery trenches, etc.
The information also can be used for general
reconnaissance, and as a screening technique
when large areas are being evaluated that have
little or no information available on past waste
disposal practices. For information on soil gas
sampling as it relates to the evaluation of vapor
intrusion, see the DoD Vapor Intrusion Handbook.
In many circumstances, soil gas sampling alone
may not be adequate to determine the source and
extent of contamination, and sampling of other
environmental media may be necessary. Soil gas
sampling should be designed to obtain all necessary information with a minimal expenditure of
time and resources. Sampling strategies are
developed by the project team to address projectspecific data needs that are identified during the
systematic planning process. Sampling strategies
will vary based on the intended purpose of the
Chapter 4 Soil Sampling

soil gas survey. The overall effectiveness of a


soil gas sampling method to depict subsurface
conditions accurately is dependent on several
factors. These factors include soil permeability
and the presence of any underground obstacles or
other features affecting sampling pathways, the
nature and concentration of contamination and
the presence of interfering chemical compounds,
and infiltration moisture and barometric pressure
changes.
Sampling considerations include site physical
constraints, soil types and stratigraphy, and background information available. Multiple depth
sampling should be considered when complex
geologic settings are encountered. Sample locations also must account for a variety of physical
properties of the soil, including grain size, cohesiveness, organic matter, moisture content, geographic fractures, and overall soil permeability.
Not all of these properties may be known in
advance, but a review of any background information such as past sampling or well installation
should be accomplished prior to soil gas sampling. If this information is not available, it may
be beneficial to install a continuously cored boring to the proposed greatest depth of the soil gas
investigation and examine the soil lithology.
Low permeability materials may result in a lower
flow rate for active sampling and passive sampling may be a better choice. It may also be
necessary to install an increased number of sampling points in low permeability soil to achieve
sufficient coverage, or reevaluate the need for
that particular sampling location.
In addition, the properties of the chemical contaminants must also be considered, including volatility, solubility or immiscibility in water, and
degradation potential. Soil gas sampling technology is most effective in mapping low-molecularweight, halogenated, or aromatic hydrocarbons
that possess high vapor pressures and low
aqueous solubilities (e.g., benzene, toluene, trichloroethylene, vinyl chloride, etc.). Rainfall or wet
soil conditions decrease the porosity of the soil
and limit diffusion of contaminants. Soil gas
sampling should not be performed after a rainfall
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event. Barometric pressure changes can introduce atmospheric air into the shallow vadose
zone, so soil gas should not be sampled during
the passing of a weather front. All of the factors
listed above can affect the ability of contaminants
to be properly sampled. In most cases, adjustments to the sampling strategy can be made to
increase sampling effectiveness.
When soil gas sampling is used to optimize monitoring wells or soil boring locations or monitor
the integrity of USTs, a sampling strategy based
on a judgmental or biased approach is recommended. However, when soil gas sampling is
used for general site reconnaissance, the use of a
statistical sampling method (i.e., a systematic grid
approach) is typically used. Many projects use a
combination of these sampling strategies. For
instance, an initial sampling may be done by a
predetermined regularly spaced grid pattern to
identify the presence of contamination, followed
by a judgmental or close, irregularly spaced grid
pattern approach to refine the delineation of the
contamination detected. Grid spacing shape and
size should be based on the project objectives and
allowable uncertainty in the decision-making
process, but be flexible enough to allow modifications in the field to account for site characteristics, or generated results.
Soil gas samples may be generated in conjunction
with an active or passive sampling system. An
active soil gas sampling system involves the
forced movement of bulk soil gas from the vadose zone to a collection device through a probe
or similar apparatus by the influence of a vacuum
source. The air within the system may be monitored real-time through a sample port with an
appropriate detector (e.g., photoionization detector (PID) or flame ionization detector (FID)).
Active soil gas systems may also be sampled with
a gas-tight syringe, Tedlar bags, glass bulbs,
Summa canisters, or other containment devices
for subsequent onsite or off-site analyses.
The active soil gas sampling system may also be
configured to collect a sorbent sample. In this
type of system, the probe is connected to a collecChapter 4 Soil Sampling

tion device designed to extract and trap chemical


contaminants from the soil gas stream by adsorption. The collection medium is dependent on the
contaminant being collected and is typically
activated charcoal, silica gel, activated alumina,
various porous polymers, or molecular sieve
adsorbents that have been prepared by thermal (or
solvent) desorption treatment. Using sorbent
media is especially useful when contamination is
present that is below the instrument sensitivity
capabilities for whole air samples, and preconcentration of the contaminants onto the adsorbent can be accomplished by passing a large
volume of air past the sorbent and trapping the
contaminants of interest. Some sorbent media
can also be used to segregate interfering compounds (e.g., reactive or oxygenated organic
compounds) by treating or designing the medium
so the interferences will not be adsorbed, or easily
desorbed, from the collection medium.
Sorbent samples are also beneficial when the
chemical contaminants are more amenable or
more efficiently removed and detected by extraction techniques. Limitations in the collection of
sorbent samples include interactions between the
contaminants and the sorption medium, the release of artifacts during the desorption process,
and susceptibility to high humidity, which can
significantly impact the adsorption efficiency of
the sorption medium. Advantages in using an
active soil gas sampling system include the quick
turnaround for data (a larger amount of soil gas is
sampled more rapidly), the generation of concentration-based data (mass of contaminant per
volume of air sampled) that can be used in a
contaminant transport model or risk assessment,
and the ability to tailor the survey as it
progresses. Limitations of an active soil gas
system include its increased cost compared with
that of passive techniques because of the need for
a vacuum source and additional collection
equipment. Driven probes associated with active
soil gas sampling also tend to degrade the natural
soil permeability around the body of the probe
due to soil compaction during probe insertion.

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This may severely impede the active soil gas flow


in moist, heavy clay soils.
A passive soil gas sampling system entails placing a collection device in the subsurface or on the
surface of the ground. Most commonly, passive
soil gas sampling techniques are used in conjunction with a sorbent medium. Several varieties of
these collection devices exist, with slightly different configurations. However, the basis for sampling is the same, in that it is the passive movement of contaminants in soil gas to a sorbent
medium contained in a collection device over a
specified period of time. Several types of sorption media are available, which, due to their
adsorption properties, will reduce the contaminant concentration directly adjacent to the device.
This induced concentration sink helps maintain
continuous migration of contaminants from the
vadose zone toward the collection device by
diffusion and mass transfer. The rate of contaminant migration is limited by many of the same
factors affecting the active soil gas sampling
techniques. These include soil physical characteristics and the physical and chemical properties of
the contaminants. In addition, caution must be
exercised during installation or backfilling to
avoid cross-contamination of the sorbent media.
Typical residence times for the collection devices
range from several days to weeks to complete.
Advantages to the use of a passive soil gas sampling system include its nominal cost, its lower
susceptibility to meteorological changes, and the
increased ability to detect less volatile compounds when compared with active soil gas sampling. Limitations include an extended turnaround time for data, the need for more samples
for thorough coverage because passive samplers
generally sample a smaller volume of soil gas, the
lack of concentration-based data, and it the inappropriateness for use with soil vapor extraction
system design.
Soil gas samples may be analyzed onsite, or
samples may be containerized and shipped to a
laboratory for off-site chemical analyses. Methods for preservation of whole air and sorbent
samples are relatively limited and are generally
Chapter 4 Soil Sampling

intended to retard thermal and photodegradation.


Preservation methods for whole and sorbent
samples are typically avoidance of heat or light.
This may be as simple as placing samples potentially exposed to light (e.g., Tedlar bags) in dark
plastic garbage sacks, and keeping them out of
direct sunlight. Sorbent samples preservation will
vary based on the sorbent medium used. Therefore, follow any procedures identified by the
vendor or manufacturer.
The ASTM D5314 standard provides a guideline
for setting up an active soil gas sampling system.
The California Environmental Protection Agencys Department of Toxic Substance Control also
has comprehensive guidance on active soil gas
sampling. Additional procedures may be necessary based on the manufacturers specifications.
Typically, the active soil gas sampling system
involves sampling devices that are directly inserted into the soil to be sampled without drilling/excavation using static pressure, impacts, or
vibration, or the sampling device is inserted into
the soil ahead of an auger or drill bit if performing deep sampling or vertical profiling. The
equipment generally used to drive the sample
probe is small and relatively compact allowing
for mobility around the site and access to confined areas. The probe is then retracted slightly
to remove the expendable drive point or open a
sample port and create a void where soil gas may
enter the sample probe. A vacuum is drawn on
the system with a pump to induce the flow of soil
gas through the sample probe to the surface
where whole air or sorbent samples may be acquired. There must be a good seal between the
probe and the earths surface to minimize pulling
atmospheric air into the collector. A drop in
vacuum or too low a vacuum may indicate system
problems. Sample containers may include, gastight syringes, Tedlar bags, Summa canisters,
etc., for a whole air sample. If using Summa
canisters to collect samples, ensure that the valves
have remained closed during shipping from the
laboratory and are fully functional. In some
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lated by the amount of time the valve is open,


rather than by monitoring the gauge on the flow
controller. Similarly, when collecting field replicate soil gas samples, proper flow splitters and
controllers must be used to maintain the same
flow rates to individual Summa canisters. Additionally, the soil gas may be collected on an
appropriate sorbent media and cartridge at a
location between the probe and the vacuum
pump, or analyzed by a real-time monitor such as
a photo-ionization detector or FID. Appropriate
decontamination procedures should be followed
between each soil gas sample collected.
4.6. Methods of Accessing Soils

A diagram of a typical bucket auger is provided


in Figure 4-2.
4.6.2. Subsurface Samples
Subsurface samples should consist of undisturbed
soil starting at the depth below the surface specified in the SAP. Subsurface samples should not
contain material from different layers of soil.
Collection of subsurface soil samples requires
that the overlying soil be removed. The SAP
should detail material separation and depths of
subsurface sampling, including sample mixing,
splitting, and representativeness.
Figure 4-2. Bucket Auger

It is important that soil samples consist of reasonably undisturbed soil from the specified sampling
depths. Access to the soil often requires drilling
or excavation down to the specified depth. In
some cases, it may be necessary to use a jackhammer to remove either concrete or pavement
from the sampling locations. In instances where
areas are grass-covered and no surface sample is
required, several square feet of sod should be
carefully cut away. A decontaminated stainless
steel shovel should be used to carefully remove
the turf so that it may be replaced when sampling
is complete. The stainless steel shovel should be
decontaminated between sampling locations.
Turf also can be removed by hand from sample
locations, provided that personnel wear clean
nitrile or PVC gloves.
4.6.1. Surface Samples
Soil samples should be taken from undisturbed
soil, not from material that is temporarily lying on
the ground. Unless the SAP specifically requires
the sampling of surface debris, remove organic
debris such as leaves, and accumulated trash or
demolition rubble, to expose the soil. The SAP
should define the depth of surface samples. Specific state and local compliance programs may
define surface samples as the first 3, 6, or 12
inches below the vegetation layer. Note in the
FLB/FN how much and what kind of material is
removed. Surface samples can be collected using
stainless steel trowels, spoons, or bucket augers.
Chapter 4 Soil Sampling

A variety of tools, ranging from handheld methods to larger fuel-powered methods, can be
used to access unconsolidated soils. Consolidated
soils can be difficult to sample because they are
difficult to penetrate. Different drilling methods
can be used to access consolidated soils. Truckmounted drill rigs can gain access to soil at any
reasonable depth and can penetrate hard layers.
When used with a hollow-stem auger, a drill rig
can retrieve reasonably undisturbed cores for
classification purposes. The following subsections describe the various techniques used to
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access both unconsolidated and consolidated


subsurface soils.
4.6.2.1. Augers
An auger is a hole-making tool that is screwed
into the soil; see Figure 4-3. The auger is used to
bore a hole to a desired sampling depth and is
then withdrawn. In general, augers should be
used only to gain access to the soil that is to be
sampled. Augers churn the soil and destroy its
structure, making soil classification more difficult
and causing rapid release of volatile contaminants. Also, when augers are lowered into boreholes, they can scrape soil off the sides of the
hole so samples collected from the bottom of the
hole may be contaminated with soil from shallower levels.
Figure 4-3. Augers

Table 4-1. Types of Augers


Sampling
Device
Screw
Auger
Standard
Bucket
Auger
Sand
Bucket
Auger

Mud
Bucket
Auger
Dutch
Auger

In situ Soil
Recovery
Auger

Eijkelcamp
Stony Soil
Auger
Planer
Auger

Various types of augers are available. The major


types of augers, their advantages, and their limitations are summarized in Table 4-1.

Applications

Limitations

Cohesive, soft or
hard soils, or
residues
General soil or
residue

Will not retain


dry, loose, or
granular material
May not retain
dry, loose, or
granular material
Difficult to
advance boring in
cohesive soils

Bit designed to
retain dry, loose,
or granular
material, silt,
sand, and gravel
Bit and bucket
designed to wet
silt and clay soil
or residue
Designed
specifically for
wet, fibrous, or
rooted soils
(marshes)
Collection of soil
sample in reusable liners;
closed top
reduces contamination from
caving sidewalls
Stony soils and
asphalt

Will not retain


dry, loose, or
granular material

Similar to
standard bucket
auger

Clean out and


flatten the
bottom of
predrilled holes

A hand auger can be used to expose soil as deep


as 4 feet. Gasoline-powered portable augers may
be able to reach up to 12 feet depending on soil
conditions, but are heavy, require two people to
operate, and may contaminate samples when
volatile organics are to be sampled.
The hollow-stem auger is commonly used in
unconsolidated soils. The hollow-stem auger
column rotates as it drills into the ground and is
designed to push soil up and out of the borehole
along the outside of the auger. The auger itself is
driven either mechanically or by a hydraulically-

Chapter 4 Soil Sampling

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powered drill rig. A plug is placed through the


auger to prevent soil from rising through the
hollow portion of the stem. Samples are retrieved
by retracting the plug and lowering the sample
collection tube through the auger. Casings and
screens for access holes can be placed in the
hollow stem to prevent the borehole wall from
collapsing and to ensure discrete interval samples. Casings also can be used to isolate nearsurface contamination while drilling continues
using a smaller diameter auger.
Auger Procedures
1. Clear the area to be sampled of any surface
debris, such as twigs, rocks, or litter. It may
be advisable to remove the first 3 6 inches
of surface soil from an area 1 foot in diameter
to prevent loose near-surface soil particles
from falling down the hole.
2. Attach the auger bit to a drill rod extension,
and then attach the drill rod to the T handle or
the power unit.
3. Begin drilling, periodically removing, and
depositing accumulated soils onto a plastic
sheet spread near the hole. This practice prevents accidental brushing of loose material
back down the borehole when removing the
auger or adding drill rods, facilitates refilling
of the hole, and avoids possible contamination
of the surrounding area.
4. After reaching the desired depth, slowly and
carefully remove the auger from the hole.
4.6.2.2. Direct-Push Techniques
Direct-push methods involve pushing a smalldiameter hollow steel rod into the ground to a
selected depth and can be used in most materials
that can be augered or sampled with a split
spoon. Direct-push techniques typically rely on a
truck-mounted hydraulic ram to gain access to
subsurface soils. The hydraulic ram pushes a
closed-end 2-inch diameter sampler into the
soil, down to the sampling depth. The sampler
contains a removable sampling tube and is capped
with a retractable penetrating point. After the
sampler is pushed to the desired depth, the peneChapter 4 Soil Sampling

trating point is retracted and the sampler is advanced to collect the soil sample inside the removable tube. This sampler can reach depths of
30 60 feet or more in sand or fairly loose soil,
but has trouble penetrating clay and hard materials. As with any sampling device, hydraulic
rams have both advantages and disadvantages.
The advantages of direct-push technology include
the following:

Retrieves relatively undisturbed soil cores up


to 18 inches long. By collecting cores from
different depths at closely adjacent locations, it
is possible to develop a continuous core for
soil classification purposes.
Collects samples rapidly- one core sample can
be collected every 10 minutes
Minimizes the release of organic vapors,
reducing personnel exposure hazards
Generates little to no waste soil as compared to
other drilling methods.
The primary disadvantages of direct-push technology include the following:

Requires the rental of special equipment and


trained operators
Soil cores are only inch in diameter, so
several core samples may have to be obtained
from a single sampling location to meet the
laboratory sample quantity requirements.
Direct-push technology has rapidly become the
method of choice for collection of subsurface soil
samples due to its speed and low cost. There are
currently numerous commercial environmental
drilling companies located throughout the country
that can provide direct-push soil sampling services.
4.6.2.3. Sonic Drilling
Sonic drilling is used for continuous sampling in
unconsolidated and soft/fractured bedrock. The
primary benefit of this technology is that very
rapid drilling rates, combined with reduced volumes of secondary waste, are possible. Recent
improvements in equipment design could lead to
increased use in the future. A sonic rig uses an
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oscillator or head with eccentric weights driven


by hydraulic motors to generate significant sinusoidal force in a rotating pipe drill. The frequency of vibration (generally between 50 and 120
cycles per second) of the drill bit or core barrel
can be varied to allow for the optimum penetration of subsurface materials. A dual-string assembly allows for the advancement of casing
along with the inner casing used to collect samples. Small amounts of air and water can be used
to remove the material between the inner and
outer casings. When a drill bit is used, most of
the cuttings are forced into the borehole wall. A
thin-wall or split-spoon sampler can be used to
obtain continuous samples. Sonic drilling also is
referred to as vibratory drilling and rotosonic
drilling.
4.6.2.4. Cable Tool
Cable tool drilling is well suited for areas contaminated by hazardous substances because it does
not use any circulation fluids that could potentially spread contamination. Auger drilling and
sonic drilling are the only other drilling methods
that do not use circulation fluids. Of these two,
only sonic drilling has demonstrated the ability to
contain contaminants as effectively as the cable
tool.
There are two types of cable tool drilling methods
used in the field.

Hard Tooling (Percussion Drilling). Best


used below the water table in areas where
unsaturated zone soils become consolidated.
Drive Barrel (Dry Drilling). This technique
is appropriate for relatively dry,
unconsolidated soils, such as sand and gravel,
often found in the unsaturated zone (i.e., the
soil above the water table).
Cable tool drilling rigs operate by repeatedly
lifting and dropping a heavy string of drilling
tools attached to a cable into the borehole. The
drilling string of a cable tool consists of five
components:

Chapter 4 Soil Sampling

1. Consolidated rock is broken or crushed into


small fragments, and unconsolidated material
is loosened by the drill bit or shoe.
2. The drilling stem connects the drill bit to the
drilling jars.
3. The drilling jars are used to vibrate the drill
bit free of the formation.
4. The swivel or rope socket connects the remaining drill tools to the cable.
5. The cable is strung over a pulley on the mast
to the drill motor.
Hard tooling is the most common form of cable
tool drilling and can be used in any formation,
including basalt. The percussive action (producing a noise level of 53 115 decibels) of the drill
bit crushes the formation. The cable is attached
to an eccentric walking or spudding beam that
also serves to mix the crushed or loosened particles with water (generally 10 20 gallons if no
water is present in the formation) to form slurry at
the bottom of the borehole. Periodically, the
drilling string is removed, and the slurry is pulled
from the borehole using a sand pump or bailer.
The drive barrel method uses the cable tool rig to
drive the drill casing into the soil. The soil is
pushed inside of the casing and then collected in a
split-spoon sampler or core barrel.
4.6.2.5. Test Pits
Under unusual circumstances, the excavation of a
test pit may be useful in determining the depth
and thickness of different types of soil or any
apparent band of soil contamination. A backhoe
can be used to remove sections of soil. This
method probably is the most expensive method of
accessing soils for sampling due to the relatively
high cost of backhoe operation.
Samples should be collected from undisturbed
portions of the walls or bottom of the pit, not
from soil that is excavated from the pit. Before
digging a test pit, four stakes should be driven
into the ground far enough from the sample location that they will not be disturbed by the backhoe
or other activities. The stakes should be located
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such that strings attached to opposite posts will


intersect directly above the sampling location.

- The backhoe may have to be


decontaminated before removing it
from the site
- Trench walls deeper than 3 feet may
be unstable. Shoring may be required
prior to having anyone enter the test
pit to collect samples
- Toxic or flammable vapors may
accumulate in the test pit. Any entry
into a test pit that is at least 4 feet deep
should be considered a confined space
entry, and all applicable requirements
should be imposed and detailed in the
HASP. See Section 4.4.2.3 for a brief
discussion of confined space entry
requirements.

The following procedures are used for excavating


test pits or trenches for soil sampling:

Prior to any excavation with a backhoe, it is


important to ensure that all sampling locations
are clear of overhead and buried utilities
Review the site-specific HASP and ensure that
all safety precautions, including installation of
appropriate monitoring equipment, are taken
as required
Using the backhoe, excavate a trench approximately 3 feet wide and 1 foot deep below the
cleared sampling location. Place excavated
soils on plastic sheets. Trenches greater than
5 feet deep must be sloped or protected by a
shoring system, as required by OSHA
regulations.
A shovel is used to remove a 1- to 2-inch layer
of soil from the vertical face of the pit where
sampling is to be done
Samples are taken using a trowel, scoop, or
coring device at the desired intervals. Be sure
to scrape the vertical face at the point of
sampling to remove any soil that may have
fallen from above and expose fresh soil for
sampling. In many instances, samples can be
collected directly from the backhoe bucket if
the soils in the bucket are representative of the
target sampling location.
Abandon the pit or excavation according to
applicable state regulations. Generally,
shallow excavations can be backfilled with the
removed soil material.
The advantages of excavating test pits include the
following:

Visibility. Provides the best information on


the location of soil layers.
Versatility. May be the only way to access
subsurface soil where large rocks are present.
The disadvantages of excavating test pits include
the following:

Safety

Chapter 4 Soil Sampling

Note: Excavation of contaminated soil can lead to the


vaporization of toxic chemicals or the generation of contaminated dust, posing an inhalation hazard to sampling
personnel. The SAP and HASP should address these
potential hazards.

Environmental
- If soil contamination is suspected,
large quantities of soil may have to be
put into containers such as drums and
stored or disposed of as hazardous
waste
- If the pit is refilled with excavated
soil, contaminated surface material
may be buried to a greater depth, or
contaminated soil from subsurface
layers may be exposed on the surface.

4.6.3.

Subsurface Geological/Geotechnical
Characterization
There are several drilling techniques that can be
utilized to characterize the subsurface geology of
a site. These drilling techniques do not provide
undisturbed soil samples and should not be used
in place of sonic drilling or cable tool methods.
4.6.3.1. Direct Mud Rotary
The direct mud rotary technique provides a flexible and rapid drilling method for a wide range of
borehole diameters in consolidated and unconsolidated materials. Direct mud rotary drilling uses
a rotating drill pipe with a hard-tooled drill bit
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attached at the bottom. Fluid is forced down


through the drill pipe and then back up the borehole. The fluid is then discharged at the surface
through a pipe or ditch into a sedimentation tank,
pond, or pit. As the cuttings settle in the pond,
the fluid overflows into a suction pit, where a
pump recirculates the fluid back through the drill
rods. The drilling fluid serves to accomplish the
following:

Cool and lubricate the bit


Stabilize the borehole wall
Prevent the inflow of formation fluids, thus
minimizing cross-contamination of aquifers.
Casing is not required during drilling. When
unconsolidated materials overlie a bedrock aquifer, mud rotary can be used to drill the bedrock.
The hole can then be cased and a less intrusive
drilling method, such as air rotary, can be used to
complete the borehole. Reverse-circulation
rotary drilling is a variant of the mud rotary method in which drilling fluid flows from the mud
pit down the borehole outside of the drill rods and
passes upward through the bit. Cuttings are
carried into the drill rods and discharged back
into the mud pit. Reverse-circulation rotary
drilling equipment is similar to direct mud rotary
drilling equipment except that most pieces are
larger.
4.6.3.2. Directional Drilling
Directional drilling technology has the potential
to offer borehole access to subsurface areas beneath buildings, tanks, landfills, and impoundments, where vertical drill rigs cannot reach.
Directional drilling involves the use of equipment
located at the surface to drill slanted or horizontal
holes into the subsurface. Test applications have
focused primarily on remedial activities, but the
potential exists for use during characterization
and monitoring activities. All directional drilling
systems require the following:

A steerable drill stem


The capability to detect the location of the drill
head or trajectory of the borehole.

Chapter 4 Soil Sampling

Directional drilling equipment ranges in size from


scaled-down rigs developed for the oil industry to
relatively compact, simple equipment used to
install utilities.
4.6.3.3. Direct Air Rotary with Rotary
Bit/Down-Hole Hammer
Direct air rotary drilling should be considered for
all situations involving consolidated rock. Air
rotary drilling relies on a sharp bit to drill through
earth and rock layers. A system of cables, engines, support mechanisms, lubricating devices,
and pulleys control the rotation of the bit below
the surface, keep the bit lubricated, and bring
debris out of the borehole. The basic rig setup for
air rotary with a tri-cone or roller-cone bit is
similar to the setup for direct mud rotary drilling,
except the circulation medium is air instead of
water or drilling mud. Compressed air circulates
down through the drill rods to cool the bit and
then carries cuttings back up the borehole (a
minimum 6-inch diameter hole required) to the
surface. A cyclone separator is used to slow the
air velocity and allow the cuttings to fall into a
container. Several different bits might be used on
a single borehole when drilling deep through
different layers of rock. A larger diameter bit is
generally used at the start of the drilling process
with progressively smaller bits used to finish the
hole. Use of a down-hole hammer in place of a
roller-cone bit provides better penetration in hard
geologic formations.
4.6.3.4. Rotary Diamond Drilling
Rotary diamond drilling is used for borehole
drilling and coring in consolidated rock. This
method uses a rotating bit consisting of a tube
that is 10 26 feet long, with a diamond-studded
ring fitted to the end of the core barrel. Water is
circulated through the bit to cool the cutting
surface. The diamond bit cuts through rock, with
a solid core remaining in the tube.
4.6.4. Use of Soil Sampling Equipment
Soil sampling equipment should be selected
according to the objectives of the sampling program. It is important to determine the depth at
which samples will be collected prior to the start
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of a sampling program because sample depth will


determine the types of equipment required. All
sampling equipment should be decontaminated
prior to use at each sampling location. Decontamination should be conducted in a controlled area
before entering the site. Equipment should be
decontaminated in the field between sampling
locations as described in Section 4.9.
Note: Sampling equipment suppliers listed in EPAs
manual Description and Sampling of Contaminated Soils A Field Pocket Guide can be contacted to obtain pictures
and information on soil sampling equipment.

4.6.4.1. Trowels, Scoops, and Spoons


Small hand tools can be used to collect surface
samples and samples of undisturbed soil from the
sides and bottoms of sampling pits. These small
tools also are used to mix and handle soil obtained from deeper locations.
A trowel is a small shovel. A laboratory scoop is
similar to a trowel, but the blade is usually more
curved and has a closed upper end to contain the
soil. Scoops come in different sizes and makes.
Many are chrome plated, but these are unacceptable, since the plating can peel off and contaminate
the soil sample. Stainless steel scoops are preferred. However, scoops made from other materials may be acceptable in certain instances.
Stainless steel trowels and scoops can be purchased from scientific or forestry equipment
supply houses. Stainless steel spoons can be
purchased from housewares departments.
Hand tools should be decontaminated and
wrapped in aluminum foil prior to use. If the
equipment is not pre-wrapped in aluminum foil or
another clean wrap material, sampling personnel
should assume that it is not clean and should not
use it.
4.6.4.2. Tube Samplers
Tube samplers are hollow tubes that are driven or
screwed into the soil. The soil fills the tube and
is retained when the sampler is withdrawn. Various types of tube samplers are available. The
applications and limitations of the various types
are summarized in Table 4-2. The split-spoon
Chapter 4 Soil Sampling

sampler and Veihmeyer sampler are discussed in


Sections 4.6.4.3 and 4.6.4.4.
4.6.4.3. Split-Spoon Sampler
A split-spoon sampler is a length of carbon or
stainless steel tubing split along its length and
equipped with a drive shoe and drive head. Splitspoon samplers are available in a variety of
lengths and diameters and generally are used to
collect undisturbed soil cores of 18 or 24 inches
in length. A series of consecutive cores may be
extracted with a split-spoon sampler to give a
complete soil column profile, or an auger may be
used to drill down to the desired depth for sampling. If an auger is used, the split spoon is then
driven to its sampling depth through the bottom
of the augured hole and the core extracted. A
standard 2-foot split spoon is advanced ahead of
the auger with a 140-pound hammer. Due to its
weight, the split-spoon sampler is generally used
with a drill rig. The advantages of split-spoon
samplers include the ability to be driven into hard
soils and the ease of extraction of the soil sample. When split-spoon sampling is performed to
gain geologic information, all work should be
performed in accordance with ASTM D1586,
Standard Test Method for Penetration Test and
Split-Barrel Sampling of Soils.
Split-spoon samplers are available typically in
diameters of 2 3 inches. A larger barrel may
be necessary to obtain the required sample volume.
Split-Spoon Sampler Use Procedures:
1. Use an auger or drill rig to open a borehole
down to the depth to be sampled.
2. Assemble the split-spoon sampler by aligning
both sides of the barrel, and then screw the
drive shoe with retainer onto the bottom and
the heavier head piece onto the top.
3. Place the sampler in a perpendicular position
to the sample material.
4. Using a well ring, drive the tube. Do not
drive past the bottom of the head piece, or
compression of the sample will result.
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5. Record the length of the tube used to penetrate the material being sampled and the number of blows required to obtain this depth.
6. Withdraw the sampler, and open it by unscrewing the bit and head and splitting the
barrel. The amount of recovery and the soil
type should be recorded.

ommended for core sampling of most types of


soil; however, it may not be applicable to sampling stony, rocky, or very wet soil. A basic
Veihmeyer sampler is shown in Figure 4-4 and
contains the following components.
Figure 4-4. Veihmeyer Sampler

Table 4-2. Types of Tube Samplers


Sampling
Device
Split-spoon
Sampler

Soil Probe

Shelby
Tubes

Soil
Recovery
Probe

Veihmeyer

Peat
Sampler

Applications
Disturbed
samples from
cohesive soil

Cohesive, soft
soils or residue;
representative
sample in soft to
medium cohesive soils and silts
Cohesive, soft
soils or residue;
special tips for
wet or dry soils
are available
Similar to thinwalled tube;
cores are collected in reusable
liners, minimizing contact
with the air
Cohesive soils or
residue to depth
of 3 meters

Limitations
Ineffective in
cohesionless sands;
not suitable for
collection of
samples for
laboratory tests
requiring
undisturbed soil
Sampling depth
generally limited to
less than one meter

Similar to
Veihmeyer tube

Similar to
Veihmeyer tube

Difficult to drive
into dense or hard
material; will not
retain dry, loose or
granular material;
may be difficult to
pull from the
ground

Wet, fibrous
organic soils

4.6.4.4. Veihmeyer Sampler


The Veihmeyer sampler was developed by Professor F. J. Veihmeyer of the University of California at Davis. The Veihmeyer sampler is recChapter 4 Soil Sampling

Tube, 1.5 meters (5 feet)


Tube, 3 meters (10 feet)
Drive head
Tip
Drop hammer, 6.8 kilograms (15 pounds)
Puller jack and grip, recommended for deep
soil sampling.
The Veihmeyer sampler can achieve substantial
depths with appropriate lengths of tubing, and
various heads are available for different soil
types. However, the Veihmeyer sampler can be
difficult to clean, and some sampler components
are constructed of materials that are not approved
for the collection of certain types of analytes.
Veihmeyer Sampler Use Procedures
1. Assemble the sampler by screwing the tip and
the drive head onto the sampling tube.
2. Insert the tapered handle (drive guide) of the
drive hammer through the drive head.

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3. Place the sampler in a perpendicular position


to the material to be sampled.
4. With one hand holding the tube, drive the
sampler into the material to the desired sampling depth by pounding the drive head with
the drive hammer. Do not drive the tube further than the top of the hammers guide.
5. Record the length of the tube that penetrated
the material being sampled and the number of
blows required to obtain this depth.
6. Remove the drive hammer, and fit the keyhole-like opening on the flat side of the hammer onto the drive head. In this position, the
hammer serves as a handle for the sampler.
7. Rotate the sampler at least two revolutions to
shear off the sample at the bottom.
8. Lower the sampler handle (hammer) until it
just clears the two ear-like protrusions on the
drive head, and rotate about 90 degrees.
9. Withdraw the sampler by pulling the handle
(hammer) upwards. When the sampler cannot
be withdrawn by hand, as in deep sampling,
use the puller jack and grip.
10. Dislodge the hammer from the sampler, turn
the sampler tube upside down, tap the head
gently against the hammer, and carefully recover the sample from the tube.
4.6.4.5. Thin-Wall Open Tube Samplers
Thin-walled core samplers are most commonly
used for collection of undisturbed core samples in
cohesive soils, silt, and sand above the water
table. Sample collection procedures are similar to
those for split-spoon sampling except that the
tube is pushed into the soil using the weight of
the drill rig, rather than driven. Some common
thin-wall open tube samplers are discussed below.
4.6.4.5.1. Shelby Tube
Shelby tube samplers are used to obtain undisturbed samples in cohesive soils, silt, and sand
above the water table. A Shelby tube consists of
a thin-walled tube with a tapered cutting head.
The device allows the sampler to penetrate the
Chapter 4 Soil Sampling

soil and aids in retaining the sample in the tube


after the tube is advanced (without excessive
force) to the desired depth. A Shelby tube is used
mainly for collecting geologic information but
may be used to obtain samples for chemical
analysis.
Shelby tube samplers are easily cleaned, and
VOC samples can be sent to the laboratory within
the tube, thus minimizing air exposure. However,
Shelby tube samplers can be difficult to drive into
hard soils and are not durable in rocky soils.
Further, certain types of soils can be difficult to
extract from the tube.
Shelby Tube Sampler Use Procedures
1. Use an auger or drill rig to open a borehole
down to the depth to be sampled.
2. Place the sampler over the borehole in a
perpendicular position.
3. Push the tube into the soil by a continuous
and rapid motion, without impact or twisting.
In no instance should the tube be pushed further than the length provided for the soil sample.
4. Let the tube sit for a few minutes to allow
soils to expand in the tube.
5. Before pulling out the tube, rotate it at least
two revolutions to shear off the sample at the
bottom.
6. If the sample is to be shipped for geologic
analysis, the ends of the tube should be sealed
with wax to preserve the moisture content. In
such instances, the procedures and preparation for shipment should be in accordance
with ASTM D1586-83.
4.6.4.5.2. Continuous Tube
Continuous tubes are similar to Shelby tubes,
except that the longer barrel is designed to operate inside the column of a hollow-stem auger.
Continuous Tube Sampling Procedures
1. Use an auger or drill rig to open a borehole
down to the depth to be sampled.

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2. Remove the auger from the drill rods, and


insert a pre-cleaned thin-wall tube sampler.
Install the proper cutting tip (an optional step
is to first replace the auger tip with a planer
auger to clean out and flatten the bottom of
the hole before using the tube sampler).
3. Carefully lower the tube sampler down the
borehole. Gradually force the tube sampler
into the soil. Do not scrape the borehole
sides. Avoid hammering the rods, because
the vibrations may cause the boring walls to
collapse.
4. Remove the tube sampler, and unscrew the
drill rods.
5. Remove the cutting tip and the core from the
device.
6. Discard the top of the core (approximately 1
inch) because it possibly represents material
collected before penetration of the layer of
concern. Place the remaining core into the
sample container(s).
7. If another sample is to be collected from a
greater depth in the same hole, reattach the
auger bit to the drill and assembly, and follow
steps 2 through 7, making sure to decontaminate the auger and tube sampler between
samples.
8. Abandon the hole according to applicable
state regulations. Generally, shallow holes
can be backfilled with the removed soil material.
4.6.4.5.3. Thin-Wall Piston/Specialized
Thin-Wall Tube
Thin-wall piston samplers usually are used when
soil conditions are unfavorable for conventional
thin-wall samplers. Piston samplers are similar to
conventional thin-wall samplers except they are
equipped with internal pistons to generate a vacuum within the sampler as it is withdrawn from
the soil. Many specialized thin-wall piston samplers have been developed for collecting undisturbed samples of a wide variety of soil types, as
exemplified below:
Chapter 4 Soil Sampling

Internal Sleeve Piston. Heaving sands (used


with a hollow-stem auger)
Wireline Piston. Cohesive soils and noncohesive sands (used with a hollow-stem
auger)
Fixed-Piston. Cohesive soils, silts, and sand
above or below the water table
Stationary Piston, Free Piston, and Open
Drive. Undisturbed samples in stiff cohesive
soils. Representative samples in medium to
soft cohesive soils, silts, and sands.
The various types of specialized thin-wall tube
samplers (and the soil types they are designed to
collect) are listed below:

Pitcher. Undisturbed samples in hard


cohesive soils and cemented sands.
Representative samples in soft to medium
cohesive soils, silts, and sands. Frequently
ineffective on loose soils
Denison. Undisturbed samples in hard
cohesive soils, cemented sands, and soft
rocks. Not suitable for undisturbed sampling
of loose or soft cohesive soils
Vicksburg. Similar to Shelby tube but able to
sample denser, coarser material.
4.7. Soil Sampling Procedures
The procedures described here generally apply to
any type of soil sampling. Any departures from
the procedures contained in the SAP should be
documented and justified.
4.7.1. Preparation
Thorough preparation is the key to a successful
project. Before beginning any sampling program,
personnel should complete the following:

Review the SAP and HASP to identify special


equipment and procedures
Obtain the required equipment. A sample list
of soil sampling equipment is provided at the
end of this chapter
Inspect the site to ensure that present
conditions are the same as indicated in the

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SAP and that all designated sample locations


are accessible
Prepare decontamination facilities for
personnel and equipment as required by the
HASP.
Refer to Chapter 3 for a complete discussion of
sampling preparation requirements applicable to
all types of sampling programs.
4.7.2. Sample Collection
Field sampling personnel should be familiar with
all of the technical issues and documentation
provided in the SAP. The following sampling
procedures can be used when there are no special
conditions present or special requirements specified by the SAP. Refer to Chapter 3 for a complete discussion of sample collection requirements applicable to all types of sampling programs.
4.7.2.1. Surface Samples
The simplest and most direct method for collecting surface soil samples is with a spade and
scoop. The accuracy and representative nature of
these samples depends on the care and precision
demonstrated by the sampler. A flat, pointed
trowel can be used to cut a block of soil 2 inches
deep. Chrome plated tools, common with garden
implements such as potting trowels, should be
avoided.
Sampling Procedures
1. Clear the area to be sampled of any surface
debris such as twigs, rocks, and litter. Cut
grass down to the level of the soil and remove.
2. Define a sample area such that a 2-inch deep
soil sample will provide enough material for
all required sample containers.
3. Dig a trench at least 2 inches deep around the
sample block using a clean spade.
4. Cut the sample loose from the ground using a
pre-cleaned stainless steel trowel. Place the
soil in a clean stainless steel bowl.

Chapter 4 Soil Sampling

5. Remove all roots and other debris. Describe


the amount and kind of material removed in
the FLB/FN.
6. If instructed by the SAP, sieve the sample as
described in Section 4.7.4.2.
7. Fill the sample container(s).
4.7.2.2. Subsurface Samples
Handheld augers and thin-walled tube samplers
can be used separately or in combination to collect subsurface samples. Where rocky soils do
not limit the use of tube samplers, a combination
of augers to remove soil material to the depth of
interest and tube samplers for actual sample
collection allows the most precise control of
sample collection. Depths of up to 2 meters can
be readily sampled, and depths of up to 6 meters
can be achieved where conditions are favorable.
A drill rig should be used to gain access where
deeper samples are required or where soil conditions preclude the use of augers. Tables 5-1 and
5-2 summarize the applications and limitations of
different types of augers and tube samplers for
sampling under different soil conditions. Section
4.6.2.1 describes procedures for using augers.
Section 4.6.4.5 discusses the selection and use of
various types of thin-walled tube samplers.
4.7.2.3. VOCs
EnCore samplers can be used to collect soil
samples for VOC testing. Separate procedures
are provided below for collecting samples with
high and low concentrations of VOCs.
Note: The EnCore sampler has not been thoroughly
evaluated by EPA as a sample storage device. While
preliminary results indicate that storage in the EnCore
device may be appropriate for up to 48 hours, samples
collected in this device should be transferred to the soil
sample vials as soon as possible, or analyzed within 48
hours.

When sampling for VOCs, soil samples should be


taken from auger cuttings only if soil conditions
make collection of undisturbed cores impossible.
New techniques, such as direct-push technologies
with the ability to continuously measure vadose
zone VOC concentrations in the soil gas, are
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useful for defining the boring depth where discrete soil samples should be collected for laboratory analysis. Soil recovery probes with dedicated or reusable liners (see Table 4-2) will minimize contact of the sample with the atmosphere.
Sampling Procedures
Low-Concentration VOC Soil Samples
Steps 1 5 are performed prior to transporting
VOC vials to the field for sample collection.
1. Add approximately 1 gram of sodium bisulfate to each vial. If samples that are markedly
smaller or larger than 5 grams are to be collected, adjust the amount of preservative to
correspond to approximately 0.2 grams of
preservative for each gram of sample.
Enough sodium bisulfate should be present to
ensure a sample pH of 2.
2. Add 5 milliliters of organic-free reagent water
to each vial. The water and the preservative
will form an acid solution that will reduce or
eliminate the majority of the biological activity in the sample, thereby preventing biodegradation of the VOAs.
3. Seal the vial with the screw cap and septum
seal. If double-ended, fritted vials are used,
seal both ends as recommended by the manufacturer.
4. Affix a label to each vial to eliminate the need
to label the vials in the field. This will ensure
that the tare weight of the vial includes the label. The weight of markings added to the label in the field is negligible.

7. Add about 5 grams (2 3 centimeters) of soil


from the EnCore Sampler to the sample vial containing the preservative solution. Quickly brush any soil off the vial threads, and immediately seal the vial with the septum and
screw cap. Store samples on ice at 6C.
Note: When samples are known or suspected to contain
high levels of carbonates, a test sample should be collected,
added to a vial, and checked for effervescence. If a rapid or
vigorous reaction occurs, discard the sample and collect
low-concentration samples in vials that do not contain the
preservative solution.

8. When practical, use a portable balance to


weigh the sealed vial containing the sample to
ensure that 5.0 0.5 grams of sample were
added. The balance should be calibrated in
the field using an appropriate weight for the
sample containers. Record the weight of the
sealed vial containing the sample to the nearest 0.01 gram.
High-Concentration VOC Soil Samples
1. Add 10 milliliters of methanol to each vial.
2. Seal the vial with the screw cap and septum
seal.
3. Affix a label to each vial to eliminate the need
to label the vials in the field. This will ensure
that the tare weight of the vial includes the label. The weight of markings added to the label in the field is negligible.
4. Weigh the prepared vial to the nearest 0.01
gram, record the tare weight, and write it on
the label.

5. Weigh the prepared vial to the nearest 0.01


gram, record the tare weight, and write it on
the label.

Note: Vials containing methanol should be weighed a


second time on the day that they are to be used. Vials
found to have lost methanol (reduction in weight of > 0.01
gram) should not be used for sample collection.

6. Using an EnCore Sampler, collect approximately 5 grams of sample as soon as possible


after the surface of the soil or other solid material has been exposed to the atmospheregenerally within a few minutes at most. Carefully wipe the exterior of the sample collection device with a clean cloth or towel.

5. Using an EnCore Sampler, collect approximately 5 grams of sample as soon as possible


after the surface of the soil or other solid material has been exposed to the atmospheregenerally within a few minutes at most. Carefully wipe the exterior of the sample collection device with a clean cloth or towel.

Chapter 4 Soil Sampling

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6. Add about 5 grams (2 3 centimeters) of soil


from the EnCore Sampler to the sample vial containing the preservative solution.
Quickly brush any soil off the vial threads,
and immediately seal the vial with the septum
and screw-cap. Store samples on ice at 6C.
7. When practical, use a portable balance to
weigh the sealed vial containing the sample to
ensure that 5.0 0.5 grams of sample were
added. The balance should be calibrated in
the field using an appropriate weight for the
sample containers. Record the weight of the
sealed vial containing the sample to the nearest 0.01 gram.
4.7.2.4. Other Parameters
Collect approximately one liter of soil for each
sample, and follow procedures for sampling
handling and preparation (see Section 4.7.4).
Record the depth from the surface to the top and
the bottom of the core, soil color, type, and other
attributes in the FLB/FN. If the sample consists
of two different types of soil (e.g., sand and clay,
or different color layers), split the core as required so that only one soil type is present in the
sample; record the depth of the change of soil
types in the FLB/FN.
Following sample preparation and handling, cap
sample bottles tightly, affix labels, and place the
bottles in resealable plastic bags. The chemical
preservation of soils generally is not required.
However, samples should be cooled to 6C as
soon as possible.
4.7.3. Composite Sampling
Compositing is the process of physically combining and homogenizing several individual soil
aliquots. Compositing provides for an average
concentration of contaminants over a certain
number of sampling points, which reduces both
the number of required laboratory analyses and
the sample variability. Compositing always
should be implemented with caution. Composite
samples should be collected only after full justification and documentation of rationale in the
sampling plan. Composite sample collection
Chapter 4 Soil Sampling

techniques should not be used if justified solely


on the basis of reducing sample testing costs.
The method of compositing the sample should be
documented and uniform to ensure future data
comparability.
4.7.3.1. Composite Sampling Techniques
If composite samples are collected, the first step
is to collect a soil sample from the sampling
location specified in the sampling plan using the
documented procedure. Any variation from the
stated procedure or SAP must be recorded. Composite samples may be collected on the basis of
biased sampling or a variety of statistical sampling techniques. Biased sampling is used when
visual, odor, or volatile organic detection is
found. A portion of the material is collected and
combined with other positive areas. Two statistical sampling techniques that can be used for
composite sampling are described below.
4.7.3.1.1. Random Sampling
Random sampling is the arbitrary collection of
samples within defined boundaries of the area of
concern. Random sample locations should be
chosen with a random selection procedure (e.g.,
using a random number table). Each sampling
point must be selected independently, so that all
locations within the area of concern have an equal
chance of being selected. Randomization is
necessary to support probability or confidence
statements about the sampling results. The key to
interpreting these probability statements is the
assumption that the site is homogeneous with
respect to the parameters being monitored. The
random sampling technique will not adequately
characterize the true conditions of a heterogeneous site.
The following example illustrates how random
soil sampling has been used to verify the
achievement of soil remediation objectives:
Random Sampling Example. Approximately
300 tons of diesel contaminated soils were excavated from a railroad fueling operation and thinly
spread over approximately one half acre to allow
for biodegradation. A single composite soil
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sample was to be collected quarterly for total


petroleum hydrocarbons to monitor remedial
progress. The composite sample was to be prepared from 6 discrete soil samples. To collect the
6 soil samples from random locations across the
half-acre area, a grid consisting of 40 equally
sized squares was placed on a site map showing
the area. Each square was numbered from 1 40,
and a random number generator was used to pick
locations from the grid. The sampling team then
collected discrete soil samples from each of the
six locations and prepared a single composite
sample for laboratory analysis.
4.7.3.1.2. Stratified Random Sampling
Stratified random sampling often relies on historical information and prior analytical results (or
screening data) to divide the sampling area into
smaller areas called strata. Each stratum is more
homogeneous than the site as a whole. Strata can
be defined based on various factors, including
sampling depth, contaminant concentration levels, and contaminant source areas. Stratified
random sampling imparts some control upon the
sampling scheme but still allows for random
sampling within each stratum. Different sampling approaches may be selected to address the
different strata at the site. Stratified random
sampling is a useful and flexible design for estimating the pollutant concentration within each
depth interval or area of concern.
4.7.3.2. Sample Compositing Procedures
In most cases of sample compositing, equal
amounts of material are collected and mixed in
the sample container. Protocols for combining
the sample are based on site conditions, the parameters being measured, the regulatory limit, and
DQOs. The rationale for the use of glass, stainless steel, or polyethylene equipment for combining samples, and the rationale for combining the
soil in equal amounts, proportional amounts, or
other amounts should be documented.
Specify the method for selecting the composite
aliquots and the compositing factor in the sampling plan. The compositing factor is the number
of aliquots to be composited into one sample
Chapter 4 Soil Sampling

(e.g., 3 1, 10 1). Determine this factor by


evaluating the detection limits for parameters of
interest and comparing them with the selected
action level for that parameter. Compositing also
requires that each discrete aliquot be the same in
terms of volume or weight and that the aliquots
be thoroughly homogenized. Because compositing dilutes high-concentration aliquots, the applicable detection limits should be reduced accordingly. If the composite value is to be compared
to a selected action level, then the action level
should be divided by the number of aliquots that
make up the composite to determine the appropriate detection limit (e.g., if the action level for a
particular substance is 50 parts per billion (ppb),
an action level of 10 ppb should be used when
analyzing a 5-aliquot composite). The detection
level need not be reduced if the composite area is
assumed to be homogeneous in concentration (e.g.,
stack emission plume deposits of particulate contamination across an area, or roadside spraying of
waste oils).
In an example situation of a soil sampling program designed to detect petroleum products in an
area of homogenous concentration, an appropriate
sample compositing technique would be to use an
adequately sized resealable freezer storage bag.
Sampling personnel would collect a minimum of
three equally sized samples (10 is preferred) from
designated sample locations and place those
samples in the sample bag. Personnel would then
close and secure the bag using care to eliminate
trapped air and combine the samples by tumbling
and kneading until fully mixed.
Soil samples should be homogenized after compositing is complete to ensure soil uniformity.
Note: Do not composite or mix soil samples that are to be
tested for volatile organics.

4.7.4. Sample Handling and Preparation


Proper sample handling and preparation ensures
that each sample container is filled with soil that
represents the entire sample and that large rock
fragments are either removed or included in each
container in an amount proportional to their
presence in the soil, as specified by the SAP.
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Techniques for sample handling and preparation


are provided in the subsections below.
4.7.4.1. Soil Homogenization
Homogenization is the mixing or blending of a soil
sample to provide uniform distribution of contaminants. Ideally, proper homogenization ensures
that portions of the containerized samples are
equal or identical in composition and representative of the total soil sample collected. Incomplete
homogenization will increase sampling error.
Samples to be composited or split should be homogenized after all aliquots have been combined.
Manually homogenize samples using a stainless
steel spoon or scoop and a stainless steel bucket, or
use a disposable scoop and pan.
Note: Do not homogenize soil samples that are to be tested
for volatile organics.

4.7.4.2. Sieving
Sieving eliminates large rock fragments. Under
some EPA protocols, only fine soil material
should be analyzed; see Figure 4-5 for an illustration of sieves.
Note: Do not sieve soil samples that are to be tested for
volatile organics.

Instructions for sieving are as follows:


1. Break up soil aggregates and pull apart any
vegetation and root mat, if present. Weigh
the non-soil vegetation fraction, and archive
or discard, as required by the SAP.
2. Remove and weigh large rocks. Archive for
possible analysis.
Figure 4-5. Sieves

3. Crush the entire soil sample with a rolling pin,


stainless steel spoon, or similar tool. Mix thoroughly with a stainless steel spoon.
4. For samples of surface soil, sieve through a
clean 0-mesh (No. 1, 2 mm) screen. Use a
3/8-inch standard sieve (9.5 mm) to screen
samples that will be tested to determine
whether the soil should be classified as hazardous waste under RCRA. Use a disposable stainless steel screen for samples to be
analyzed for semivolatile organic contamination. Use Teflon screens for samples to be
analyzed for metal contamination.
5. If the soil is too wet or too cohesive to pass
through the sieve, note that the required sieving was not done in the FLB/FN, and enter
this notation on the Field Sampling Form. Inform the Sampling Program Manager that the
sample could not be sieved.
6. Spread out the screened sample, mark off
quarters, and take samples from each quarter
in a consecutive manner until appropriate
sample volume is collected. If specified, archive the remaining sample for future analysis.
7. Before shipping the samples to the laboratory,
shake each sample container to mix thoroughly.
4.7.4.3. Splitting Samples
Many times samples are split between representatives of the property owner or between state or
federal enforcement agencies so results may be
independently verified. Soil samples split between laboratories are typically performed to
evaluate laboratory quality. Soil samples should
be split from a single sampling event following
homogenization and sieving. Specific procedures
for splitting samples for VOC, semivolatile organic, and metal analyses are described below.

Chapter 4 Soil Sampling

Splitting Samples for VOC Analysis. To


split samples for VOC analysis, collect two
core samples from adjacent locations.
Alternatively, split a soil core longitudinally
with a clean knife and place half of the core
into each sample container, minimizing air
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contact as much as possible. The method of


splitting the sample may greatly affect the
results. Documentation and execution of the
splitting technique should be uniform to ensure
data comparability.
Splitting Samples for Semivolatile Organic
Chemical (SVOC) and Metal Analyses. To
split samples for semivolatile and metal
analyses, place the soil in a clean stainless steel
bowl. Crush and thoroughly mix the soil with
a clean stainless steel spoon. Document the
method used for sample mixing and placing
into the sample containers to ensure data
comparability. One method is to form mixed
soil into a cone and divide in half vertically.
Each set of sample containers is then filled
with the soil from half of the pile.
4.8. Restoration of Sample Locations
Sample locations should be restored to eliminate
tripping hazards and remove conduits for contaminated runoff to reach subsurface soils. Take
precautions to prevent introducing contaminated
soil into uncontaminated soil horizons or leaving
contaminated soil exposed on an otherwise clean
surface.
4.8.1. Backfill Sample Holes
Soil pits and boreholes should be backfilled after
samples have been collected. For shallow pits
and boreholes where only one soil horizon is
involved, the Sampling Program Manager may
deem it appropriate to backfill with material from
the pit or hole if this action has been specified in
the SAP.
If backfilling with removed material is not authorized by the SAP, or where more than one soil
horizon is involved, the pit or borehole should be
backfilled with clean soil or sand. The fill material should be added in layers no more than 6
inches thick. Each layer should be compacted
before more soil is added. This procedure will
minimize subsequent settling.
4.8.2. Grouting Boreholes
Boreholes that penetrate a confining layer (e.g.,
silt, clay, or rock that acts as the base of an aquiChapter 4 Soil Sampling

fer) should be grouted to prevent migration of


contaminated water between aquifers. Grouting
consists of filling the borehole with concrete or
bentonite slurry as specified by the Sampling
Program Manager and the SAP. Record grouting
details (e.g., depth of borehole, depth to confining
layer, mix ratio, and amount of the grout used) in
the FLB/FN for each borehole.
4.8.3. Replace Sod
Sod should be replaced in grass areas after the
boreholes and pits are filled. The sod originally
removed from the area should be used if it is still
alive. Otherwise, commercial sod can be used or
the area should be seeded, depending on the
requirements of the facility.
4.8.4. Replace Pavement
Areas of pavement that were removed to obtain
access to soil should be repaired after the pit or
borehole is filled. As required by the facility, the
patch may be cold patch asphalt, hot asphalt, or
concrete.
4.9. Decontamination
It is generally not possible to have a separate set
of precleaned stainless steel sampling equipment
for each sample if significant numbers of samples
are to be collected. Sampling equipment should
be decontaminated prior to use to prevent contaminants from being transferred from one sample
to the next. If sampling equipment must be
reused, it must be decontaminated prior to sampling and between each sample location.
All field decontamination should take place on a
decontamination pad lined with plastic. Solvent
rinse liquids must be collected in dedicated containers. All aqueous decontamination liquids
should be stored in DOT approved compatible
containers (e.g., 55-gallon drum or appropriate
size). If nitric acid is used to rinse the sampling
equipment, the rinse liquids should be neutralized
by adding lime to each drum (1 cup of slaked
lime, Ca(OH)2, per drum). If any hazardous
chemical is used on site, the SAP must detail
proper waste material handling procedures.

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Decontamination Solutions and


Supplies
Decontamination equipment, materials, and
supplies are generally selected based on availability. Other considerations include the ease of
decontaminating or disposing of the equipment.
Most equipment and supplies can be easily procured such as softwash and rinse solutions. Childrens wading pools also can be used. Large
plastic garbage cans or other similar containers
lined with plastic bags can help segregate contaminated equipment. Contaminated liquid can be
stored temporarily in metal or plastic cans or
drums. The following standard materials and
equipment are recommended for decontamination
activities:

- Acetone (pesticide grade), hexane


(pesticide grade), and methanol, only
if sample is to be analyzed for
organics.

4.9.1.

Solutions
- Non-phosphate detergent
- Selected solvents such as acetone,
hexane, nitric acid, and isopropyl
alcohol
- Dilute bases
- Tap water
- Distilled or deionized water.
Tools and Supplies
- Long and short handled brushes
- Bottle brushes
- Drop cloth or plastic sheeting
- Paper towels
- Plastic or galvanized tubs or buckets
- Pressurized water sprayers
- Solvent sprayers
- Aluminum foil
- Trash bags
- Trash containers
- 55-gallon drums
- Metal or plastic buckets or containers
for storage and disposal of
decontamination solutions.
Solvent Rinses
- 10% nitric acid is typically used for
inorganic compounds such as metals.
An acid rinse may not be required if
inorganics are not a contaminant of
concern.
Chapter 4 Soil Sampling

Note: All cleaners or solvents must be approved by the


Program Manager or designee. At least once a day, collect
samples of the cleaner and water that have been used as a
final rinse for the equipment for submission to the laboratory as an equipment rinsate blank.

Table 4-3 provides a summary of the solvent


types and recommended solvent rinses for various
types of pollutants.
Table 4-3. Soluble Contaminants and Recommended Solvent Rinse
Solvent1
Water

Dilute
Acids

Dilute
Bases

Organic
Solvents2

Examples of
Solvents
Deionized water,
tap water.

Soluble
Contaminants
Low-chain hydrocarbons, inorganic
compounds, salts,
some organic
acids, and other
polar compounds.
Nitric acid Acetic Basic (caustic)
acid, boric acid.
compounds (e.g.,
amines and
hydrazines).
Sodium bicarboAcidic comnate (e.g., soap
pounds, phenol,
detergent).
thiols, some nitro
and sulfonic
compounds.
Alcohols, ethers
Nonpolar comketones, aromatics, pounds (e.g., some
straight-chain alka- organic comlines (e.g., hexane), pounds).
common petroleum
products (e.g., fuel,
oil, kerosene).
Hexane
PCBs

Organic
Solvents2
1
Material Safety Data Sheets (MSDSs) are required for all
decontamination solvents or solutions as required by the
Hazard Communication Standard.
2

WARNING: Some organic solvents can permeate or


degrade protective clothing.

4.9.2. Procedure
The following procedures should be used to clean
field sampling equipment between samples. Note
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that different procedures are used depending on


whether the equipment will be used to collect
samples for metals or organic analysis and the
level of detection required for the compliance
program. Cleaning and decontamination procedures for equipment used to collect soil samples
for analysis for organic and inorganic chemicals
are as follows:

Segregate Equipment Drop


- Place plastic sheeting on the ground.
Size will depend on amount of
equipment to be decontaminated.
- Provide containers lined with plastic if
equipment is to be segregated.
Segregation may be required if
sensitive equipment or mildly
contaminated equipment is used at the
same time as equipment that is likely
to be heavily contaminated.
- Deposit equipment used on site (e.g.,
tools, sampling devices, and
containers, monitoring instruments
radios, etc.) on the plastic drop cloth
or sheet, or in different containers with
plastic liners. Each will be
contaminated to a different degree;
segregation at the drop reduces the
probability of cross contamination.
- Loose leaf sampling data sheets or
maps can be placed in plastic zip lock
bags if contamination is evident.
Physical Removal With a High-Pressure
Washer (Optional)
- A high-pressure wash may be required
for compounds that are difficult to
remove by washing with brushes. Hot
water from the high-pressure washers
is excellent at removing greasy or oily
compounds.
- High-pressure washers require water
and electricity
- A decontamination pad may be
required for the high-pressure wash
area. An example of a wash pad may
consist of an approximately 1-footdeep basin lined with plastic sheeting
Chapter 4 Soil Sampling

and sloped to a sump at one corner. A


layer of sand can be placed over the
plastic, and the basin is filled with
gravel or shell.
- The sump is also lined with plastic,
and a barrel is placed in the hole to
prevent collapse. A sump pump is
used to remove the water from the
sump for transfer into a drum.
- Heavy machinery is usually
decontaminated at the end of the day
unless site sampling requires the
machinery be decontaminated more
frequently. A separate decontamination pad may be required for heavy
equipment.
- Use high-pressure wash on grossly
contaminated equipment. Do not use
it on sensitive or non-waterproof
equipment.
Physical Removal with Brushes and a Wash
Basin
- Fill a wash basin, a large bucket, or
childs swimming pool with nonphosphate detergent and tap water.
Approximately 10 50 gallons of
water may be required initially
depending upon the amount of
equipment to decontaminate and the
amount of gross contamination.
- Scrub equipment with soap and water
using bottle and bristle brushes
- Only sensitive equipment (e.g., radios,
air monitoring and sampling
equipment) which is waterproof
should be washed
- Equipment that is not waterproof
should have plastic bags removed and
wiped down with a damp cloth
- Acids and organic rinses may also ruin
sensitive equipment. Consult the
manufacturers for recommended
solutions.

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Equipment Rinse
- Fill a wash basin, a large bucket, or
childs swimming pool with tap
water. Approximately 10 50 gallons
of water may be required initially
depending upon the amount of
equipment to decontaminate and the
amount of gross contamination.
- Rinse soap off equipment with water
by immersing the equipment while
brushing. Repeat as many times as
necessary.
Low-Pressure Rinse
- Fill a low-pressure sprayer with
distilled or deionized water during the
rinsing process. Approximately 10
20 gallons of water may be required
initially depending upon the amount of
equipment to decontaminate and the
amount of gross contamination.
- Rinse sampling equipment with
distilled or deionized water with a
low-pressure sprayer.

Note: Personal protective equipment (PPE) recommended


for handling nitric acid includes nitrile gloves, boot covers,
rubber apron or coated Tyvek coveralls, and eye protection (e.g., face shields or goggles).

Nitric Acid Sprayers (Required Only if


Metals Are a Contaminant of Concern)
- For low-level contamination or where
equipment rinsate blanks demonstrate
metals contamination, rinse stainless
steel equipment with 10% nitric acid
(trace metal or higher grade HNO3
diluted with distilled or deionized
water)
- Fill a spray bottle with 10% nitric
acid. An acid rinse may not be
required if inorganics are not a
contaminant of concern. The amount
of acid will depend on the amount of
equipment to be decontaminated.
- Provide a 5-gallon bucket or basin to
collect acid during the rinsing process
- Rinse sampling equipment with nitric
acid. Begin spraying (inside and

Chapter 4 Soil Sampling

outside) at one end of the equipment


allowing the acid to drip to the other
end into a 5-gallon bucket.
Low-Pressure Sprayers
- Fill a low-pressure sprayer with
distilled or deionized water during the
rinsate process.
- Rinse sampling equipment with
distilled or deionized water with a
low-pressure sprayer.
Organic Solvent Sprayers
- Fill a spray bottle with an organic
solvent. After each solvent rinse, the
equipment should be rinsed with
distilled or deionized water and air
dried. Amount of solvent will depend
on the amount of equipment to dedecontaminate.
- Provide a 5-gallon bucket or basin to
collect the solvent during the rinsing
process
- Solvent rinses may not be required
unless organics are a contaminant of
concern
- Rinse sampling equipment with a
solvent. Begin spraying (inside and
outside) at one end of the equipment
allowing the solvent to drip to the
other end into a 5-gallon bucket.
- Allow the solvent to evaporate from
the equipment before going to the next
step. A QC rinsate sample may be
required.
Low-Pressure Sprayers
- Fill a low-pressure sprayer with
distilled or deionized water. Use a 5gallon container to collect water
during the rinsate process.
- Rinse sampling equipment with
distilled or deionized water with a
low-pressure washer.
Clean Equipment Drop
- Lay a clean piece of plastic sheeting
over the bottom plastic layer. This
will allow easy removal of the plastic
in the event that it becomes dirty.
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- Provide aluminum foil, plastic, or


other protective material to wrap clean
equipment
- Lay clean equipment on plastic
sheeting. Let air dry, wrap sampling
equipment with aluminum foil, plastic,
or other protective material.
Record Information
- Information concerning
decontamination methodology, date,
time, and personnel should be
recorded in the FLB/FN.
4.9.3.

Preparation of Equipment Rinsate


Blanks
Equipment rinsate blanks provide a check on the
cleanliness of sampling equipment and the purity
of the water or solvent used for the final rinse(s).
See Chapter 3 for information on collecting
equipment rinsate blanks.
At least one equipment rinsate blank should be
submitted each day for each type of rinse solvent
used (e.g., water, acetone). The SAP should
specify the size and material of each sample
bottle required for equipment rinsate blanks and
any required preservatives for these liquid samples.
Equipment rinsate blanks consisting of solvents
such as acetone or hexane will be classified as
flammable liquids and will require special packaging (in metal cans). Special labeling and manifesting requirements apply for shipments of
flammable liquids sent to the lab by common
carrier.
4.10. Waste Material Storage and Disposal
All material generated during soil sampling
projects should be stored as hazardous waste until
disposal decisions are made based on generator
knowledge or test results. This includes soil
cuttings, equipment decontamination wastes, and
used disposable PPE.
4.10.1. Soil Cuttings
Soil cuttings from boreholes and test pits may be
classified as hazardous waste and should thereChapter 4 Soil Sampling

fore be containerized and stored in accordance


with EPA and facility requirements. Soil cuttings
must not be used to fill the boreholes or test pits
unless specifically authorized by the SAP or
regulatory authority.
Soil cuttings should be placed on plastic sheets
when generated. The soil should be stored in
metal drums that are marked to indicate the
source of the contents. The plastic sheets should
be disposed with the used PPE.
4.10.2. Used Disposable PPE
All disposable solid contaminated equipment
(e.g., plastic sheets, screens, coveralls, boot covers, etc.) should be placed in plastic bags temporarily, then sealed in metal barrels for final storage, transport, and disposal based on generator
knowledge or test results.
4.11. Sampling Equipment List
Section 3.8 provides a generic sampling equipment list applicable to most sampling events. The
following list provides additional equipment
applicable to soil sampling. In most cases, only a
portion of the equipment listed below would be
required for a given sampling event.

Equipment for accessing soils


- Backhoe
- Augers
- Drill rigs
Soil sampling equipment
- Trowels, scoops, and spoons
- Split-spoon sampler and hammer to
advance.
- Veihmeyer soil sampler outfit
- Shelby tube
- Continuous tube
- Thin-wall tube sample
- EnCore sampler
Additional equipment
- Maps and plot plan
- Survey equipment or GPS to locate
sampling points
- Survey stakes or flags

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- Decontamination supplies and


equipment
- Canvas or plastic sheet
- Shovel (to refill sampling holes)
- Stainless steel mixing bowl
- Detergent
- Acetone, hexane, or biodegradable
organic cleaner
- Nitric acid
- Tap water
4.12. References

- Distilled or deionized water (ASTM


Type II)
- Storage and disposal containers for
wash water, acid, solvents, and soil
cuttings
- Lime to neutralize nitric acid wastes,
- Grouting materials such as concrete or
bentonite slurry
- Tape to measure sample depth
- Vermiculite.

1 ASTM D5314 Standard Guide for Soil Gas Monitoring in the Vadose Zone2 California
Environmental Protection Agency, Department of Toxic Substances Control, Advisory Active Soil
Gas Investigation, April 2012,
http://www.dtsc.ca.gov/SiteCleanup/upload/VI_ActiveSoilGasAdvisory_FINAL_043012.pdf
3 DoD Vapor Intrusion Handbook, http://www.clu-in.org/download/char/dodvihdbk200901.pdf
4 USACE Sample Collection and Preparation Strategies for Volatile Organic Compounds in Solids,
October 1998

Chapter 4 Soil Sampling

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Chapter 5. Aquatic Sediment Sampling


5.1. Purpose
This chapter provides general guidelines and
procedures for sampling approaches, methods, and
equipment for aquatic sediment characterization to
assess risks at DoD sites. This chapter provides
general guidance, and references appropriate
detailed sampling approaches, methods, and
equipment. Topics include sampling method
selection; sediment manipulation methods to
prepare for chemical analysis and toxicity testing;
sampling of sediment pore water; and sampling of
benthic invertebrate infauna (organisms that burrow in sediment (e.g., clams, worms)) and epifauna (organisms living on sediment surface and
freely roaming, (e.g., some insects and crabs)).
Key references for additional information are
provided at the end of each section.
5.2. Scope
Aquatic sediments consist of particles of mineral
or organic material that accumulate under surface
water. The particles, which include solids and
sludges that are suspended or settled in the water,
are derived from rocks or biological materials that
are either transported by flowing water bodies or
situated beneath a static aqueous layer. Sediment
types are classified by particle size, mineralogy,
source materials, and site-specific variables.
Sediment and sediment-related sampling and
analysis is used to address risk to human health or
the environment. Specific uses of sediment data
include the following:

Characterizing extent of contamination or risk


associated with site and ambient conditions
Determining impacts to benthic communities
Evaluating toxicity through bioassays
Estimating bioaccumulation of certain chemicals
Evaluating impacts from pore water
Evaluating impacts from sediment disturbance
(e.g., currents, dredging, prop-wash and
scour).

Chapter 5 Aquatic Sediment Sampling

Some sediment sampling procedures may need to


be modified to accommodate site conditions and
equipment or logistic limitations (e.g., depth to
sediment, difficulty of penetration of sediment).
Field sampling should be conducted in accordance with appropriate federal, state, or local
government regulations.
Sediment samples may be collected from streams,
lakes, ponds, creeks, lagoons, surface impoundments, and coastal (marine/estuarine) waters, near
the surface, or at deeper intervals. Benthic invertebrate collections are typically done at the surface or at shallow depths where organisms reside,
and result in benthic community measures that
may be used to compare to a reference or ambient
community in order to determine whether the site
sediments are impacted. Bioassay and bioaccumulation methods may be used to expose representative aquatic organisms to sediment, usually
in a laboratory setting, to determine their response in comparison to a reference or ambient
sediment response. Sediment pore-water sampling is also an option to determine risk of contaminants, or to assess the movement of groundwater through sediment in a groundwater discharge zone or hyporheic zone of flow.
5.3. Project Planning for Sediment-Related
Sampling
As discussed in Chapter 2, the systematic planning process is critical to acquiring representative
samples. However, sediment sampling introduces
additional concerns. For example, sediment
typically has low-level contaminant action levels
compared to waste and soil media, and related
problems with introducing trace-level crosscontamination from the bulky mechanical gear
required for sampling. Clear and concise objectives should be identified to define the intent of
the sediment-sampling program. The overall
process includes the following steps:
5.3.1. Identify Project Goals
A key step in identifying project goals is to specify the problem and indicate decisions that need to
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be made regarding it. A CSM is used to compile


and summarize existing information and hypotheses regarding contaminant sources and migration pathways to prospectively-exposed human
and environmental receptors. In many cases
regarding sediments, the prospective impacts to
these receptors is the decision. However, legal
considerations may also be important (e.g., state
laws specifying sediment cleanup requirements,
or federal or state laws that establish hazardous or
dangerous waste categories).
CSMs should consider the following as they
influence the site decisions. Table 5-1 below
shows an expanded list.

Historical site use including known or suspected contamination in site media


Site topographic and meteorological features,
including water depth and sediment thickness
The hydrodynamic conditions of the water
body as related to physical sediment fate and
transport, (e.g., runoff, current and deposition
patterns, upwelling, and seepage patterns)
Processes that influence the transport and
concentrations of contaminants present (e.g.,
advection, dilution, sediment transport, biodegradation, and dispersion)
The human and fish or wildlife utilization of the
site (e.g., children accessing sediments on
beaches, or wildlife consuming fish from the
site)
Processes that affect contaminant bioavailability.

5.3.2. Determine Data Needs


The project planning team should identify key
inputs or data needs and provide narrative statements of how data will be used in decisions, i.e.,
data quality objectives. An important part of this
process is the boundaries (spatial or temporal) of
the study, which affect the scope of the investigation.
Typical decisions for sampling sediment include
the following:

Identifying contamination presence and extent


Identifying sources of contamination
Chapter 5 Aquatic Sediment Sampling

Identifying whether contamination levels


suggest adverse biological effect
Identifying trends
Establishing goals for sediment remediation
Evaluating possible effects of dredged or fill
material discharge.
For determination of adverse biological effects,
there are several possible phases of inquiry and
response, and the process selected should be
described in the data quality objectives. What
follows summarizes the process.
5.3.2.1. Develop a Screening-Level Chemical
Evaluation
Develop a Screening-Level Chemical Evaluation
that compares site sediment and/or fish/shellfish
tissue concentrations to background and screening criteria in order to generate a list of contaminants of potential concern (COPC), and to determine whether additional investigations or actions
are needed. Until recently, sediment screening
has been based on bulk sediment concentrations
compared to database-derived measures of effect
(e.g., the National Oceanographic and Atmospheric Administration (NOAA) Screening Quick
Reference Table (SQuIRT) values), or equilibrium-partitioning derived values that estimate
the proportion of a substance in sediment pore
water. Recently, researchers have developed
better screening criteria that incorporate bioavailability as a predictor of toxicity and bioaccumulation. The National Research Council (NRC
2003) defines bioavailability processes as, individual physical, chemical, and biological interactions that determine the exposure of plants and
animals to chemicals associated with soils and
sediments. Traditional methods to assess the
potential effect of sediment contamination on
human or ecological health use total bulk sediment contaminant concentrations. However,
abundant research has shown that only a fraction
(the bioavailable fraction) of an environmental
contaminant may be taken up and may subsequently result in an effect on an organism; and
that this concentration is often much less than the
bulk concentration of these contaminants in the
sediment.

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Depending upon the project decision and the


complexity of the investigation, bioavailability
measures may be desirable to include in the
investigation. An example bioavailability screen
for divalent inorganic compounds is to collect
data on acid volatile sulfides and simultaneously
extracted metals. An example for neutral organic
compounds is to use a method for collection of
sediment pore water. Table 5-1 summarizes a
variety of measures that affect bioavailability, and
related measures that may require inquiry.
5.3.2.2. Characterize Exposure and Effect
Characterize Exposure and Effect using the
COPCs identified, and conducting human health
or ecological risk assessment, and determining
the risk or hazard associated with the sediment.
This step may also include comparisons of benthic communities of invertebrates at the site to a
reference area community as a measure of effect.
In Table 5-1, the rows titled, Evaluate Ecological and Human Health Pathways and Endpoints
apply to this step.
5.3.2.3. Assess Risk Management
Assess Risk Management options regarding the
site; these may lead to no action, or to a sediment
removal, or in the case of sites managed under
CERCLA, as amended, to a Feasibility Study and
Record of Decision (ROD) regarding the extent
of a response action.
5.3.3. Develop Data Collection Options
Specific considerations that may influence data
collection strategies for sediments may include:
Hydrologic information (e.g., runoff, current
and deposition patterns, upwelling, seepage patterns)
Water depth
Thickness and type of sediment, especially
regarding sediment grain size, as it affects
sampling efficiency and sample representativeness
Anthropogenic and natural loading (proximity
of outfalls, seasonal patterns, relevant previous
monitoring information)
Contaminant bioavailability

Chapter 5 Aquatic Sediment Sampling

Type of benthic community being represented,


as it affects the size and number of samples required for characterization; note that habitat
structure and function may influence the community composition
Potential for release of sediment chemicals to
surface water via diffusion or advection
Fate of sediment (e.g., lithic structure, current
regime with regard to depositional and erosional conditions, and related activities such as
dredging).
Specific measurements may include:

Chemical data on bulk sediment and pore


water
Sediment toxicity (organism response)
Tissue bioaccumulation (tissue levels upon
exposure to sediment)
Bioavailability measures
Benthic community analysis (e.g., habitat
structure, and benthic surveys). Although this
chapter is limited to sediment and associated
invertebrate communities, there are benthic
fish species whose life cycles are coupled to
sediment that may also be useful bioindicators.
Examples include mummichog, sheepshead
minnow, and oyster toadfish.

Table 5-1 below illustrates a range of activities


and measures potentially associated with developing project objectives and data needs. Note that
some of these evaluations and investigation methodologies are beyond the scope of this chapter,
but are potential additional lines of evidence.
Appendix B of US EPAs Methods for Collection, Storage, and Manipulation of Sediments for
Chemical and Toxicological Analyses (Ref. 1)
illustrates some typical data quality objectives
and measurement quality objectives for sediment
investigations.

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Table 5-1. Approaches Used to Assess Bioavailability of Chemicals for Sediment.


(Adopted from ITRC 2011.) The added phrase as appropriate to the site is intended to indicate that not all
sites require this evaluation.
Scoping Element

Review Site
History

Source of Information

Activity

Bioavailability Related Analyses/


Considerations

Review Available Data


(e.g., hazard ranking
documents)

Establish site boundaries,


identify adjacent facilities
Identify initial COPC
Identify geochemical parameters
Understand reference (background) conditions

Nature and extent of COPCs and exposure


COPC mobility forms and pathways
Data gap analysis (organic carbon, acid volatile
sulfides and simultaneously extracted metals,
redox, salinity, pH)

Groundwater Data, as
appropriate to the site

Understand direction and flow


Understand hyporheic zone
mixing, if present

Flux measures in sediments via piezometers,


direct pore water, or passive samplers

Assess bulk sediment

Analyses of COPC, total organic carbon, acid


volatile sulfides and simultaneously-extracted
metals, metals speciation as appropriate, and
grain size

Assess pore water,


as appropriate to the site

Sample and analyze COPC via piezometers,


direct pore water measurement by extraction or
by passive samplers
Estimate pore water fraction by Equilibrium
Partitioning, acid volatile sulfides and simultaneously-extracted metals, the biotic ligand
model, or other appropriate model(s)

Assess diffusive flux,


as appropriate to the site

Analyses of dissolved COPC immediately


above sediment/water interface, as appropriate
to the site
Estimate flux based on models, such as the
USACE RECOVERY model, a contaminated
sediment-Water interaction model

Assess Flood or ice scour,


as appropriate to the site

Estimates and/or analyses of COPC desorption


from resuspended sediments

Sediment Data
Identify Site
Transport
Processes

Potential Sediment
Hydraulics

Assess wave/current-induced
resuspension, as appropriate to Redeposition of contaminated sediment
the site
Assess boat propeller wash,
as appropriate to the site

Chapter 5 Aquatic Sediment Sampling

Measures of total and dissolved COPCs, TOC


and DOC estimates and/or analyses of COPC
desorption from resuspended sediments

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Scoping Element

Source of Information

Bioavailability Related Analyses/


Considerations

Activity

Assess resuspension flux,


as appropriate to the site

Resuspension of contaminated sediment


Exposure to buried contaminated sediments
Non-equilibrium conditions for organics
Oxidation of metals
Direct measures of COPCs in overlying waste
and newly exposed sediments
Changes in oxidation conditions
Changes in salinity; estuarine/tidal wedge
Estimates and/or analyses of COPC desorption
from resuspended sediments

Ecological receptorbased information

Plant tissue residue analysis, plant bioassays


Community analyses, bioassays, tissue residue
analysis, Equilibrium Partitioning and BiotaEvaluate receptor and exposure Sediment Accumulation Factor uptake models
pathways
Tissue residue analysis (COPC and lipid),
Biota-Sediment Accumulation Factor (BSAF),
Benthic invertebrates
kinetic uptake models
Fish and water column
invertebrates
Tissue residue analysis (COPC and lipid), oral
Wildlife
dose models, laboratory bioassays, field as Plants
sessment of fecundity
Animal testing for bioavailability (e.g., swine);
tissue residue measure (COPC and lipid), oral
dose models, laboratory bioassays

Human Health-based
information

Water analysis for COPCs, partitioning variables (e.g., Octanol-Water Partition Coefficient (Kow)), oral dose
Evaluate receptor and exposure
In-vitro/in-vivo testing for bioavailability (e.g.,
pathways:
swine oral and dermal dose models); bulk
Direct contact
sediment analysis, partitioning measures ,
Ingestion
Tissue residue(s), fraction of COPC available
for uptake (bioaccessibility),
Identification of ingestion rates

Evaluate
Ecological and
Human Health
Pathways and
Endpoints

For more information on project planning for


sediment-related sampling, consult the following
references:

Methods for Collection, Storage, and


Manipulation of Sediments for Chemical and
Toxicological Analyses: Technical Manual
(Ref. 1)
Guidance Manual to Support the Assessment
of Contaminated Sediments in Freshwater
Ecosystems Volume I - An Ecosystem-Based
Chapter 5 Aquatic Sediment Sampling

Framework for Assessing and Managing


Contaminated Sediments (Ref. 2)
Contaminated Sediment Remediation
Guidance for Hazardous Waste Sites (Ref. 3)
Implementation Guide for Assessing and
Managing Contaminated Sediment at Navy
Facilities (Ref. 4)
Critical Issues for Contaminated Sediment
Management (Ref. 5).

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5.4. Developing a Sampling Strategy


This section describes development of data collection options, and finalizing the data collection
program. Development of a sampling strategy for
purposes of characterizing a sediment site should
follow the fundamentals of the scientific approach, including appropriate quality control and
quality assurance.
Factors such as physical site constraints, safety,
and cost may influence sampling strategies.
Project strategies should consider the current and
potential future phases of an investigation, and
select the methodologies appropriate to these
phases. A phased investigative approach can
be used to refine the CSM and address the data
quality objectives for the investigation. It is
important to consider exit strategies should the
data indicate that further investigation is unnecessary. For example, comparison to conservative
bulk sediment screening values or background
comparisons are often used to determine the need
for later stages of investigation. Should the
screening values or background values be exceeded, intensified sampling could be initiated to
identify or delimit a source area and release
pattern, and to confirm whether the site concentrations represent site-related contamination.
Alternatively, a data collection program may be
more comprehensive in the first phase, for example, when contamination is believed to be present,
the source study and release pattern may occur at
the beginning of the project.
Reference locations may be important for contaminant screening, or later in the process, for
determining project-relatedness of sediment
chemistry or risk. Selection of a sediment reference location requires matching sediment characteristics (e.g., grain-size ranges, TOC, pH, eH,
and, where toxicity testing is desired, toxicity
limits) from an unimpacted or non-site reference
location to the site sediments. A reference site
selection study should define what is intended:
either a pristine reference (natural or nonanthropogenically affected reference) or a site
that represents the conditions in the watershed
apart from the site being investigated (ambient
Chapter 5 Aquatic Sediment Sampling

or anthropogenically-affected reference). In
most DoD site investigations, the latter is desired;
in some state programs, the former is mandated.
To assure that grain-size, TOC, and eH conditions
are comparable may require sampling several
stations to achieve an acceptable match. Performance criteria for reference stations should be
included in project plans. Sampling intensity at
the reference station should also be sufficient to
establish a statistically valid comparison between
it and the investigation site.
Advanced methods to determine whether receptors are likely to show adverse effects, or to
elucidate release patterns and refine the CSM
with regard to contaminant mobility and bioavailability may also be included in a second or contingent phase of the investigation. Examples
include bedded sediment bioaccumulation testing,
collection of field organisms for tissue analysis,
measures of pore water, or benthic mapping
(section 5.8).
US EPA QA/G-5s
(http://www.epa.gov/quality/qs-docs/g5sfinal.pdf) provides useful guidance on statistical
sample design including numbers and types of
samples, selection of sample locations, sampling
frequency, and sampling and analytical protocols.
In addition, there are free software programs
available such as ProUCL and Visual Sample
Plan that permit estimation of numbers of samples required.
The analyte list for sediment and pore water
sampling schema should anticipate the intended
data uses. For instance, for toxicity testing, grainsize and total organic carbon are recommended;
for some analytes (e.g., organotins), bulk sediment may not be an appropriate medium and
pore-water analysis may be required. Some
analytes (e.g., mercury) have a short holding
time, which may affect the field schedule for
delivery to analytical laboratories. There are also
limitations on holding time for sediment prior to
initiating biological testing. The sampling method
and organism size to be retained from macro
invertebrate surveys should anticipate the uses of
data (e.g., taxonomic composition and mass,
species diversity measures).
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For more information on developing a sampling


strategy, consult the following references:

Methods for Collection, Storage and


Manipulation of Sediments for Chemical and
Toxicological Analyses (Ref. 1)
Sampling for Contaminants In Sediments and
Sediment Pore Water (Ref. 6)
A Compendium of Chemical, Physical and
Biological Methods for Assessing and
Monitoring the Remediation of Contaminated
Sediment Sites (Ref. 7)
Contaminated Sediment Remediation
Guidance for Hazardous Waste Site (Ref. 3)
Ocean Testing Manual Evaluation of Dredged
Material Proposed for Ocean Disposal (Ref. 8)
Inland Testing Manual: Evaluation of Dredged
Material Proposed for Discharge in Waters of
the U.S (Ref. 9)
Guide for Incorporating Bioavailability
Adjustments into Human Health and
Ecological Risk Assessments at U.S. Navy and
Marine Corps Facilities (Ref. 10)
Incorporating Bioavailability Considerations
into the Evaluation and Remediation of
Contaminated Sediment Sites (Ref. 11)
Assessment and Remediation of Contaminated
Sediments (ARCS) Program - Assessment
Guidance (Ref. 12).

5.5. Methods for Bulk Sediment Sampling


This section presents guidelines for collecting
representative sediment samples, and targets the
selection of appropriate equipment based upon a
range of site conditions such as depth of water,
depth of sediment to be sampled, and flow regimes.
Desirable attributes for sediment sampling gear
include the following:

Creates a minimal pressure wave when descending through the water


Forms a nearly leak-proof seal when the sediment sample is taken
Prevents winnowing and excessive sample
disturbance when ascending

Chapter 5 Aquatic Sediment Sampling

Allows easy access to the sample surface so


that undisturbed subsamples may be taken
Allows vertical sectioning of undisturbed
samples for profile examination
Penetration well below the desired sampling
depth is preferred to prevent sample disturbance as the device closes. A means of weight
adjustment to assure penetration depths may be
valuable.
5.5.1. Sediment Grab Sampling Methods
Grab samplers are excellent for providing quantitative data at a relatively low cost. Considerations
for selection of core versus grab samplers are
described below in Table 5-2.
Limitations of grab samplers include:

Variability among penetration depth for samples depending on sediment properties


Oblique angles of penetration which result in
varying penetration depths within a sample
Folding or disturbing the sample, resulting in the
loss of information concerning the vertical structure of benthic communities in the sediments.
Some additional things to consider when choosing
a sampler include:

Water depth
- In less than 4 m of water, with low current
conditions and smooth water, the Birge-Ekman,
petite Ponar, Ponar, Van Veen, and Peterson
mini-Shipek grabs are recommended

- For deeper waters or greater current, the Ponar or Van Veen are recommended.
Sub-sampling from sampler directly
- If sub-sampling from the sampler is desired,
the Birge-Ekman, mini-Ponar, Ponar, Van
Veen, or Shipek are recommended
- If not, a Peterson, Smith-MacIntyre, or miniShipek are recommended.
Target sample depths
- Up to about 10 cm sample depth, a BirgeEkman, Ponar, or Shipek or miniature versions of any of these are suitable
- Up to about 30 cm, a Smith MacIntyre, Van
Veen, or Petersen grabs are suitable.
Target sample volumes to meet analytical
requirements
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- Up to about 3 L, the mini Birge-Ekman, petite Ponar, or mini-Shipek samplers are suitable
- 3 10 L samples may be collected with the
Birge-Ekman, Ponar, or Petersen grabs
- Above 10 L, Smith-MacIntyre or Van Veen
grabs are suitable.

The most common surface area sampled is about


0.1 m2 in the Van Veen and Smith-MacIntyre
grabs. Van Veen and box corers are also capable
of sampling 0.06 m2, compared to hand-held
corers, which sample about 0.001 m2.

Table 5-2. Selection Criteria for Core Sampler or Grab Sampler


Use a Core Sampler if:
Characterization of contamination in deeper sediments is important
Comparison of recent surficial vs. historical deeper
sediments is needed
Reduced sediment disturbance needed
Reduced oxygen exposure needed
Sediments are soft and fine-grained.

Sampling devices such as a Ponar or VanVeen


with removable or hinged bucket covers are
preferred to allow access to the surface of the
sediment sample without loss of water or finegrained sediments. Key sample collection issues
for grab samplers include:

For Sediment Grab Samples to be Subsampled in the Laboratory. The sample should
be transferred carefully and directly into a labeled container that is made of a chemically
inert material, tightly sealed, and air excluded.
For Sediment Grab Samples to be Subsampled in the Field. Typically, the sediment is
decanted into a cleaned bowl or bag for homogenization and sub-sampling. To minimize sediment handling and artifacts of sampling for
volatiles, samples may be taken directly from
the grab.
5.5.2. Sediment Core Sampling Methods
Core samplers (corers) are used to characterize
contamination over a depth interval that includes
sub-surface sediments. They also are used to
obtain sediment samples for geological characterizations and dating, investigate the historical
input of contaminants to aquatic systems, and to
characterize the depth of contamination at a site.
Corers are an essential tool for developing threedimensional maps of sediment contamination.
Collection of subsurface layers in addition to the
Chapter 5 Aquatic Sediment Sampling

Use a Grab Sampler if:


Large sediment volumes are needed
Larger grain-size or hard sediments would hamper
use of a core
Larger surface area of surficial sediment needed
(typical for benthic invertebrate sampling).

surface layer of sediment permits evaluation of


historical or long-term impact on site conditions,
and development of site-specific sediment transport mechanisms to refine the CSM.
Selection of the most appropriate core sampler for
a sampling event is determined based on water
depth, particle size of the sediment, sediment
sample depth, volume of sediment sample required for analysis, and available lifting capacity
of the sampling platform/boat and winch equipment. Core samplers seldom are suitable for
sampling benthic macro invertebrate samples due
to the small area sampled. See Figure 5-1 for
factors to consider when selecting a core sampler.
Because of the potential for a bow wave of
sediment at the leading end of the core, resulting
in compaction and inefficient flow of the sediment into the core sampler, percent recovery
should be evaluated. Percent recovery is determined by dividing the internal recovery by the
penetration depth. Internal recovery is the depth
inside of the core tube from the top of the tube to
the surface of the sediment. Core penetration is
measured from the outside of the core. In recent
projects in the Pacific Northwest (e.g., WindWard
2006) 75 percent core recovery has been regarded
as an appropriate control limit on core recovery;
however, it is recommended that project specific
goals be determined.
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For more information on methods for bulk sediment sampling, consult the following references:

Standard Guide for Storage, Characterization,


and Manipulation of Sediments for Toxicological Testing (Ref. 13)
Guide for General Planning of Waste Sampling (Ref. 14)
Guide for Core-sampling Submerged, Unconsolidated Sediments (Ref. 15)
Standard Guide for Selecting Grab Sampling
Devices for Collecting Benthic Macroinvertebrates (Ref. 16)
Handbook of Techniques for Aquatic Sediments Sampling (Ref. 17)
Manual of Aquatic Sediment Sampling (Ref.
18)

Chapter 5 Aquatic Sediment Sampling

Methods for Collection, Storage and Manipulation of Sediments for Chemical and Toxicological Analyses: Technical Manual (Ref. 1)
Sampling for Contaminants In Sediments and
Sediment Porewater (Ref. 6)
A Compendium of Chemical, Physical and
Biological Methods for Assessing and Monitoring the Remediation of Contaminated Sediment Sites (Ref. 7)
Ocean Testing Manual Evaluation of Dredged
Material Proposed for Ocean Disposal (Ref.
8)
Inland Testing Manual: Evaluation of
Dredged Material Proposed for Discharge in
Waters of the U.S. (Ref. 9).

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Figure 5-1. Factors in Core Sampler Selection

5.6. Bulk Sediment Handling and Analysis


If a single core will be used to represent the site,
then homogenization of selected intervals and
sub-sampling should occur; but if several cores
will represent the site (e.g., when average conditions are desired, or greater volumes of sediment
are required for biological assays), then multiple
cores should be composited by depth interval. If
labile chemicals, metals with a critical oxidation
state (particularly organotins and mercury), acid
volatile sulfides, or volatile organic compounds
are of concern, a glove box to maintain anaerobic
conditions during the sub-sampling activities may
be needed. In addition, shielding against ultravio-

carbons (PAH) samples, as some of this suite of


compounds may break down. As with grab samples, inert sampling gear and mixing apparatus
should be used to avoid cross-contamination.
U.S. EPAs Methods for Collection, Storage, and
Manipulation of Sediments for Chemical and
Toxicological Analyses lists additional recommendations for suitable sample containers, mixing gear, and sample preparation.
Once received at the laboratory, handling/manipulation procedures should be designed to maintain sample representativeness in
terms of toxicity and chemistry by minimizing
procedural artifacts. Some analytical procedures
and toxicity test protocols necessitate specific
manipulations for toxicity or elutriate testing.

let light may be needed to assure the representativeness of sediment Polycyclic aromatic hydroChapter 5 Aquatic Sediment Sampling

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Note: Specific analysis methods and protocols for performance of toxicity testing are beyond the scope of this
document, but are available in the referenced literature.

A separate sample is usually taken for physical


analysis if the sample amount is sufficient. For
chemical analysis, sieving is not recommended,
as it changes sediment composition (e.g., organic
carbon). Sieving may be required to remove
organisms that could interfere with intended
biological testing. Hand-picking is recommended
for debris. Should sieving be performed, it
should be done for all samples to be tested, including control and reference sediments if the
objective of the study is to compare results
among stations.
Sediment storage for chemical analysis is typically
done at <6 C; maximum holding times before
extraction should be defined. National and regional guidance exists for maximum holding times
prior to analysis.
Manipulation and storage of sediment for toxicological testing may have special requirements.
For more information on methods for bulk sediment handling and analysis, consult the following
references:

Standard Practice for Preparation of Sediment


Samples for Chemical Analysis (Ref. 19)
Standard Test Method for Measuring the
Toxicity of Sediment-Associated Contaminants with Estuarine and Marine Invertebrates
(Ref. 20)
Standard Guide for Conducting Acute Toxicity Tests with Fishes, Macroinvertebrates, and
Amphipods (Ref. 21)
Methods for Collection, Storage and Manipulation of Sediments for Chemical and Toxicological Analyses: Technical Manual (Ref. 1)
Sampling for Contaminants In Sediments and
Sediment Pore Water (Ref. 6).

be at thermodynamic equilibrium. This makes


pore water useful for assessing contaminant
levels and associated toxicity. Pore water is often
isolated to provide either a matrix for toxicity
testing and/or to provide an indication of the
concentration and/or partitioning of contaminants
within the sediment matrix. Pore water toxicity
tests yield information not provided by solidphase, elutriate, or sediment extract tests. Pore
water toxicity testing has proved useful in sediment toxicity identification evaluations, and may
be useful for weight of evidence regarding biological availability of some contaminants. It is
critical to use the same protocol when comparing
samples to one another.
In areas of known upwelling or downwelling
groundwater flow through sediment, pore water
may also reflect the groundwater to surface water
flux conditions, and inform the CSM. Overall
considerations for pore water investigations
include mineralogy, subsurface flows, estimated
pore water residence time, pH, temperature, redox
potential, organic carbon, sulfides, and hardness
(depending upon the water and metals).
Several approaches to determine pore water
COPC concentrations are:

5.7. Methods for Collection of Pore Water


Pore, or interstitial, water may contain contaminants partitioned from the surrounding sediment.
In depositional sediments, contaminants in the
pore water and in the solid phase are expected to
Chapter 5 Aquatic Sediment Sampling

Estimate of organics from bulk sediment concentrations (equilibrium partitioning theory)


Estimate of metals bioavailability/toxicity via
the molar ratio of acid volatile sulfides to simultaneously-extracted metals, or by the biotic-ligand model
Traditional sediment collection followed by
centrifugation or core squeezing and filtration
and/or flocculation of residual particulates.
The resultant supernatant (pore water) can be
chemically analyzed or used for toxicity testing
Sampling of pore water by use of suction
devices, piezometers, or equipment such as the
Trident System and subsequent chemical
analysis or toxicity testing
In situ or ex situ placement of diffusion or
equilibrium-based samplers directly into the
sediment or extracted pore water, and measurement of either the sampler (i.e., SolidPage 5-11

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Phase Microextraction Devices (SPME), PE


and Polyoxymethylene (POM) or the liquid
contained therein (i.e., peepers). Note that
some passive methods here indicated as in situ
may also be applied in a laboratory setting.
Most sediment collection and processing methods
likely affect pore water chemistry, contaminant
bioavailability, and toxicity to some degree.
Direct methods measure pore water chemistry
and typically compare them to ambient water
quality criteria or apply toxicity testing (e.g.,
Daphnia acute toxicity testing). However, relatively large volumes of water are required for
toxicity testing. Indirect methods include
peepers, dialysis bags, and passive media that can
include binding agents in a bag with an ionpermeable hydrogel layer, or semipermeable
membrane sorptive devices. In situ collection
techniques may outperform ex situ methods for
collecting pore water, as they are less subject to
conditions introduced by sampling and extraction.
However, in situ methods typically are restricted
to waters where wading or diver activities may be
applicable, and they produce relatively small
volumes of pore water, which may not be suitable
for the investigation needs. In situ suction devices include, push-point samplers, syringes, probes,
and core-type samplers, and may be deployed
primarily in soft sediments at depths to 30 centimeters.
Chemical artifacts may occur from exposure of
interstitial water to oxygen. Ex situ bulk sediment centrifugation, pressurization, and suction
are alternatives to in situ pore water collection,
and although they may alter water chemistry, this
may be necessary when larger sample pore water
volumes are required, or when it is not logistically feasible to collect in situ samples.
Direct Pore Water Sampling. Small diameter
piezometers may be placed in sediments where
the water is shallow and the current is relatively
weak. Clusters of such instruments may measure
hydraulic head differences and provide pore
water samples from different depths for contaminant concentration profiling. Collection can be
done using peristaltic suction lift or a centrifugal
or bladder pump. Suction may cause negative
Chapter 5 Aquatic Sediment Sampling

bias for dissolved gases and volatile organics.


The pumping needs to be done at a very low rate
to avoid mixing of the zones of interest. Piezometers offer advantages over diffusion samplers
in that they can be sampled repeatedly, and they
generally do not have volume limitations. Preservation of in situ anoxic conditions is generally
not possible; however, in-line measurements of
parameters such as DO and redox potential may
be made to determine their approximate in situ
values when suction lift is not used. Some examples of pore water samplers are:

Syringes. May be used to take samples of


pore water at different depths in a sediment
profile in shallow or diver-accessible water
depths. Pore water samples are obtained by
pushing the needle to the desired depth and retracting the plunger. Syringes may not be effective in compacted sediments or gravels and
can become plugged in very fine sediments.
They generate relatively small volumes (up to
about 0.25 L) of pore water.
Push-point samplers. Useful primarily in
shallow water although they can be deployed
by a diver. They have a small diameter core
barrel with lance tip and a T type handle.
The small diameter barrel has holes drilled in
the side at the bottom to allow water to enter.
A solid plastic rod is placed in the barrel to
prevent water and sediment from entering the
sampler during pushing. When the sampling
section of the barrel has been pushed to the
target depth, the rod is withdrawn allowing
pore water to enter. The water is sampled using a peristaltic pump or, in some cases, a syringe.
Drive-point piezometers. Best for pore water
samples at greater depth below water surface,
and at greater intervals below sediment surface
than push-point samplers. Drive-point piezometers may also be useful when sediment resists penetration of push-point devices. An example device configuration follows. A drivepoint piezometer may be fitted to a drill rod,
which is driven by an impact corer using a
pneumatic hammer. The piezometer is stainless steel fitted with a bulkhead and tubing
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barb, and with a screened section (typically


#50 or 300 m mesh). Pore water may be collected using a peristaltic pump connected by
polypropylene tubing threaded through the hollow drill rod and attached to the barb fitting on
the piezometer. The piezometer is driven to
the first desired depth, and the first pore water
sample collected after purging several casing
volumes of water (e.g., four). If desired, following first collection, the piezometer may be
driven to greater depth and another pore water
sample collected following purging. For sampling at a separate location, a new, pre-cleaned
piezometer should be used.
BAT sampler probe. Consists of a tip and
housing, which is sealed with a disc containing
a flexible septum. The tip may be constructed
of porous high-density polyethylene (HDPE)
or of stainless steel to allow pore water to enter
the sampler, which is under negative pressure.
The stainless steel tip is driven to the desired
sampling depth and a stainless steel screen is
exposed that allows pore water to enter the
sample housing. A tool containing an evacuated sample vial (35 500 mL) with a septum cap and a double-ended hypodermic
needle is lowered down the push rod, and the
needle penetrates the housing septum at the
same time it penetrates the vial septum, thus
permitting pore water to enter the vial. When
the vial is full, the tool is retrieved, and the vial
is stored for subsequent analysis. Porous
HDPE filter tips are useful for assuring low
suspended solids.
Trident Probe. (Chadwick et al., 2003;
Chadwick and Hawkins 2008) is a hand- or diver-deployable direct push system that provides depth specific temperature and conductivity data. The on-board air hammer can drive
the samplers into more compacted or stiff sediments than manual methods. It provides a
better estimate where the groundwater/surface
water interface is by looking at the differences
in temperature and conductivity of the surface
water versus water at depth, and permits selection of a sampling interval.
Following collection, pore water should be transferred to sample jars with no headspace before
Chapter 5 Aquatic Sediment Sampling

shipping to the laboratory at <6 C. Transferring


of pore water into a second jar should not be
performed unless absolutely necessary. For some
chemicals, field preservation may be required.
Indirect or Passive Pore Water Samplers. These
consist of bag samplers and sorbent samplers. Bag
samplers include the following, and may be suitable for both inorganic and organic contaminants:

Peepers and Dialysis Bags. In situ diffusion


sampling methodologies that are suitable for
shallow or diver-accessible depths. They are
not standardized, and consist of small chambers with dialysis/cellulose membranes or
mesh walls containing either distilled water or
clean water of the appropriate salinity or hardness. The devices are buried in sediments and
pore water is permitted to infiltrate the sampler. Peepers are generally limited to sediment
depths of 0.2-10 cm, and generate up to 0.5 L
of pore water. They require hours to several
weeks to equilibrate with the sediment. There
may be cross-contamination issues related to
the construction materials, and biofouling may
also cause artifacts. Peepers have also been
used to expose organisms to sediments in situ.
A possible issue with the mesh peepers is infiltration of colloidal particles into the devices.
The following are samplers that are suitable for
inorganic compounds:

Diffusion Equilibrium in Thin Films (DET)


Samplers. Consist of hydrogel-immobilized
binding agents that selectively attract ionic contaminants such as calcium, magnesium, sodium,
iron, manganese, chlorine, sulfate, nitrate, alkalinity, and total CO2. They are capable of rapid
determination of flux, but they do not measure
equilibrium pore water concentrations.
Diffusion Gradients in Thin Films (DGT).
Technique uses a similar approach to DETs to
accumulate solutes on a binding agent after
passage through a diffusion layer. A binding
agent selective to the target ions in solution
(e.g., a resin such as Chelex for metals), is
immobilized in a thin layer of hydrogel separated from solution by an ion permeable hydrogel layer. Transport of ions occurs by moPage 5-13

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lecular diffusion into the binding agent. Very


rapidly, a steady-state linear concentration
gradient is established between the solution
and the binding gel, and in situ fluxes estimated.
Common features of the several of hydrophobic
organic sorbent samples follow:

Organic sorbents are designed to reach equilibrium with the freely dissolved contaminant
phase in adjacent water. Quantitative results
can be obtained because the sorbent typically
has a known equilibrium coefficient that has
been derived from laboratory calibration studies using representative compounds. Additionally, higher concentrations of contaminants
occur in the sorbent, resulting in higher sensitivity than direct porewater measurements.
The period of exposure to assure steady state
depends upon the sorbent-water partitioning
coefficient and volume of sorbent exposed to
the pore water. High sorbent-water coefficients and large volumes of sorbent take longer
for hydrophobic contaminants to equilibrate.
Assurance or adjustments for steady state may
be assessed (in order of preference) by loss of
reference compounds with known characteristics that were introduced into the sorbent prior
to placement, selection of appropriate sorbent
thickness (hence volume), or by modeling contaminant transport into the sorbent.
An advantage of some samplers is that a single
device placed vertically in sediment can be
subdivided into sectors that may be separately
analyzed to generate a concentration profile.
This use of a sorbent sampler is useful in
monitoring the effectiveness of a sediment cap.
The gradient of concentrations that occur can
be further interpreted using advective flow
modeling.
Another advantage of sorbent samplers is that
they equilibrate with truly dissolved portion of
contaminants in water, hence do not measure
colloidally-bound contaminants, do not require
measurement of dissolved organic carbon to
substantiate equilibrium partitioning calculations, and generally do not require analytical
cleanup.
Chapter 5 Aquatic Sediment Sampling

Note: Analytical cleanup may be required for sulfur compounds that interfere with PCB analysis.

Passive samplers can function as biological


surrogates (biomimetics) for a measure of
bioaccumulation of hydrophobic organic compounds.
The principal hydrophobic organic sorbent devices follow:

Semipermeable Membrane Devices


(SPMD). Consist of flat tubular low-density
polyethylene membranes containing a thin film
of a high-molecular weight lipid (triolein), and
depend upon diffusion of organic chemicals
across a semipermeable interface to the lipid.
They are used for hydrophobic organic compounds, such as PCBs, PAHs, and organochlorine pesticides. SPMDs are relatively easy to
install and may have low detection and quantitation limits. They measure pore water concentrations as a time-weighted average, as opposed to an equilibrium concentration. In an
aquatic environment, the uptake rate into an
SPMD is linear during the first 50 days, so that
the equilibrium may be estimated. An embedded tracer with a known solution rate may be
applied to the SPMD prior to deployment to
confirm the calculations by observing losses
over time.
Solid-Phase Microextraction Devices
(SPME). Disposable glass fibers approximately the diameter of a human hair, coated
with thin layers of poly (dimethylsiloxane)
(PDMS) which sorbs organic molecules such
as PAH or PCB from sediment pore water or
surface water. SPME advantages include: cylindrical geometry aids insertion in sediments
with small diameter cylindrical tools, low limits of quantitation, and the ability to profile
contamination in sediment. SPME samplers
are available that have been calibrated for
PAHs at very low levels. SPME fibers are
prepared by sequential sonication with hexane,
acetonitrile and water, and then inserted into
sediment via a push-point device with wall
perforations to permit access to pore water.
After equilibration, which typically takes 1 - 2
weeks, the fibers are withdrawn, cut into
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lengths of interest, and transferred to autosampling vials with a small volume of solvent
(e.g., 100 L), typically hexane or acetonitrile.
There are several commercially available
SPME sizes consisting of varying core size
and PDMS content in the coating. Those with
a 1000-m core are sturdy and resilient for
field use; those with a 210 m core are
somewhat less sturdy and harder to process in
the field into autosampler vials. Sorbent coats
with 30-m layers of PDMS are high capacity
and have slower uptake kinetics. A good
compromise between quick uptake kinetics
and ease of use and processing in the field is a
15 m PDMS layer on 1000 m core.
Note: Steady-state corrections are required for PCB congeners with Log Kows 6.

Polyethylene (PE) Sampler. Consists of


readily-available polyethylene (e.g., 25 m
sheets) material resembling a painters drop
cloth; these may be placed into sediment or in
surface water. PE samplers have been calibrated for PCBs, PAHs and other organic
compounds. The rectangular geometry and
pliability may require a frame for placement in
situ, and direct extraction to autosampling vials
is difficult. PE samplers have excellent detection limits, but also have high sorbent-water
partition coefficients, which suggests longer
times to steady state relative to PDMS devices.
Polyoxymethylene (POM) Sampler. Similar
to the PE sampler, and consists of readilyavailable 76 m thick rectangular strips. POM
Samplers have been used to measure sediment
pore water and landfill leachate. The rectangular geometry permits placement into sediment
primarily in the near-surface, and makes extraction to autosampling vials difficult. POM
Samplers have excellent limits of quantitation,
but high sorbent-water partition coefficients,
which slow uptake kinetics relative to PDMS.
Ex situ Pore Water Techniques. Centrifugation,
squeezing, and vacuum extraction/filtration are
commonly used. These extraction methods may
be done in the field or in the laboratory, but extraction in the laboratory just prior to analysis or
testing is preferable, so that the sample is mainChapter 5 Aquatic Sediment Sampling

tained as close to its original state as much as


possible during transport and storage.

Centrifugation of homogenized sediment


allows collection of large volumes of pore water, and may be accomplished in an anoxic atmosphere (e.g., under nitrogen gas). Samples
are typically divided among several centrifuge
tubes. Centrifugation speed may have a
marked influence on concentrations and toxicity. For toxicity testing, sediments should be
centrifuged at 104 x g for 30 minutes to remove
colloids. However, if toxicity testing of the
interstitial fluids is the objective, this may also
reduce the toxicity of the water due to the lack
of colloidal contaminants. Less centrifugal
force may be appropriate for contaminant studies.
Sediment squeezing and vacuum extraction/filtration may be accomplished by relatively low-cost mechanical devices with a filter. There are also possible effects to equilibrium partitioning, internal mixing, and electrolyte changes. EPA (2001b) recommends
application of moderate positive or negative
pressures along with electrolyte (conductivity)
monitoring during extraction. In addition, that
extraction should be performed at in situ ambient temperatures to reduce alterations to interstitial water composition that may occur at
temperatures different from ambient conditions.
For more information on methods for collection
of pore water, consult the following references:

Standard Practice for Preparation of Sediment


Samples for Chemical Analysis (Ref. 19)
Coastal Contaminant Migration Monitoring:
The Trident Probe and UltraSeep System:
Hardware Description, Protocols, and Procedures. (Ref. 22)
Monitoring of Water and Contaminant Migration at the GroundwaterSurface Water Interface (Ref. 23)
Methods for Collection, Storage and Manipulation of Sediments for Chemical and Toxicological Analyses (Ref. 1)

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Incorporating Bioavailability considerations


into the Evaluation and Remediation of Contaminated Sediment Sites (Ref. 11)
Sampling for Contaminants In Sediments and
Sediment Pore Water (Ref. 6).

5.8. Benthic Macroinvertebrate


Investigations
When conducting a sampling event to evaluate
benthic or biological activity in aquatic sediment,
specially designed sampling equipment is used to
retain the biological content in the sediment.
Sampling is typically limited to the upper 10
inches of the sediment layer, where benthic organisms are active.
The first part of the benthic macroinvertebrate
sampling section describes methods for collection. The second part describes data acquisition
and analysis.
Benthic habitats are bottom environments with
distinct physical, geochemical, and biological
characteristics. Benthic habitats vary widely
depending upon their location and depth, and may
be characterized by dominant structural features
and biological communities. Estuarine and nearshore benthic habitats can be highly diverse,
including shallow submerged mudflats and sandflats, rocky hard-bottom habitats, seagrass beds,
kelp forests, shellfish beds, rivers, creeks,
marshes, streams and coral reefs. Data on substrate type, topography, benthos, water and sediment quality, and presence or absence of toxins
are all necessary to create an accurate picture of a
habitat and associated ecological risk. Data from
the benthos field sampling or surveys provide
information on species abundance, distribution,
and biomass. They may be collected by point
sampling (grab or core), by tow (dredge, seine,
trawl or net), by capture (cages, traps) by photographic surveys, or by other methods. Field
information such as vessel type, start and end
dates; investigator, and institution/agency; station
numbers, positions and times; and equipment and
methods are reported for each survey. Environmental data reported at each sampling site may
include meteorological and sea surface conditions; surface and bottom temperature, salinity,
Chapter 5 Aquatic Sediment Sampling

and water quality; and sediment characteristics.


Biological data would include quantity of individual organisms and total weight of organisms
for each collected species.
Marine organisms are adapted to live in particular
habitats, and knowledge of these sediment characteristics can provide insight into the physiology and ecology of the organisms sampled. Benthic macroinvertebrates tend to have high site
fidelity and integrate long-term changes in ecosystems to inform sediment investigations of
impact due to contamination. Individual macroinvertebrate species have sensitive life stages that
respond to stress and integrate effects of shortterm environmental variations, whereas community composition depends on long-term environmental conditions. In addition to taxonomic
identification, benthic macroinvertebrate investigations may require knowledge of the feeding
group to which a species belongs; for example,
suspension feeders and deposit feeders. Method
selection to provide for interpreting benthic invertebrate data requires knowledge of regional patterns of species abundance. Benthic community
measures are often combined with chemistry and
toxicity data to assess sediment impacts.
Contaminants found in marine sediments may
threaten water quality, the health of aquatic organisms, and human health. Many pollutants are
highly toxic and can persist in the environment
for years. This can cause long-term health problems in marine invertebrates and fish such as
tumors, reproductive problems, and fin rot.
Environmental contaminants may also be transferred through the food web, adversely affecting
fisheries or posing a risk to human health.
The physical characteristics of the study area
including water clarity, depth, circulation, currents,
bottom topography, sediment quality, and studyarea size influence what tools may be used effectively for macroinvertebrate surveys. Bottom
characteristics may dictate the specific tools to be
used for benthic investigations, as do physical
characteristics of sediments. When a sediment
study area is flat or gradually sloping and contains
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pling is typically preferred for defining habitat


types.
As with sediment sampling, the type of benthic
macroinvertebrate sampling gear depends on the
nature of the substrate to be sampled. The sampling area should focus on the most predominant
substrate available (in many estuaries and coastal
marine areas this will be soft sediments of mud
through sand grain sizes). Sampling for sediment
biota is typically limited to the depth of sediment
where benthic organisms are active, and this is
case-specific. In slow-flowing freshwater environments, the biologically-active zone is typically
shalow; however, in flowing water and estuarine/marine environments, it may be deeper.
According to U.S. EPA, numbers and kinds of
macroinvertebrates collected by a particular grab
are influenced by the habitat and substrate type
sampled, penetration depth of the sample, the
completeness of closure of the jaws (suggesting
potential loss of sample during retrieval), and
potential washout of surface organisms due to a
shock wave associated with the sampler deployment, and stability of the sampler in particular for
high water velocities.

Birge-Ekman, Van Veen, Ponar, and SmithMcIntyre grabs are often selected for infauna
in soft substrates (river backwaters, lakes, and
low-current velocity marine/estuarine conditions). Table 5-3 below summarizes characteristics of grab samplers.
Core samplers may be used, but they sample a
very small area and volume of sediment, thus
representativeness of the community may be
insufficient; however, this depends upon the
abundance of the community, and multiple
cores may be composited to provide sufficient
area/volume. See Table 5-4 below for comparison of coring methods.
For harder substrates and particularly for
epifaunal invertebrates, seines and trawls may
be used; however, seines and trawls typically
only gather larger organisms.
In flowing water, several techniques may be
used to harvest sediment-associated biota.
See Table 5-5 below for a summary of Stream
Net Samplers used to collect organisms from
flowing water.

Regional guidance may aid in developing a plan for


benthic macroinvertebrates. For example, the Puget
Sound Estuary Program, as applied to Puget Sound,
shows the following recommendations (additional
annotations in italics):
Kind of Sampler: Modified Van Veen
Area to be Sampled: 0.1 m2
Sample Replication (when variance is important): four
to five per station
Sieve Mesh Size: 1.0 mm (note, however, that Atlantic
coast programs often use a 0.5-mm mesh screen)
Initial Sieving Location: Vessel
Use of Relaxant Chemicals: Not recommended; in
some cases relaxants will reduce body distortion of
soft-bodied creature; however relaxants my cause
some taxa to lose limbs or other features.
Use of Biological Stains: Rose Bengal
Level of Taxonomy: Species or Higher
Sampling Season: Variable

Recommendations for selection of benthic invertebrate samplers follow:


Chapter 5 Aquatic Sediment Sampling

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Table 5-3. Advantages and Disadvantages of Commonly Used Grab Samplers

Device
Orange Peel

Use
Marine waters
and deep lakes

Smith-McIntyre Deep lakes,


rivers, and
estuaries

Sample
Depth
(cm)

Sample
Volume
(L3)

0 18

10 20

Comes in a range of sizes

Need large boat, powered


winch and cable line
Blocking of jaws may
cause sample loss

0 4 (in
deep sand)

10 20

Reasonable quantitative
samples
The trigger plates provide
added leverage essential to
its penetration of substrate

Heavy, need boat and


power winch
Spring-loaded jaws,
hazardous
Inadequate for deep
burrowing organisms

Advantages

Disadvantages

Birge-Ekman,
small

Lakes and
marine areas;
soft sediments,
silt, and sand

0 10

3.4

Handles easily without


winch or crane
Can be adapted for shallow
water use
Good for soft sediments,
sand, and silt
Allows sub-sampling

Restricted to low current


due to light weight and
messenger activation
May exceed target penetration depth
Sub-sampling may be
restricted by size of top
flaps

Birge-Ekman,
large

Lakes and
marine areas;
soft sediments,
silt, and sand

0 30

13.3

Can be adapted for shallow


water use
Good for soft sediments,
sand, and silt
Allows sub-sampling

Restricted to low current


conditions
Penetration depth can
exceed desired level due
to weight of sampler
Heavy, requires winch

Ponar, standard Deep lakes,


rivers, and
estuaries; useful
on sand, silt, or
clay

0 10

7.25

May not close completely,


resulting in sample loss
Metal frame may contaminate sample
Heavy, requires winch

Ponar, petite

0 10

1.0

Most universal grab sampler


Adequate on most substrates
Large sample obtained intact,
permitting sub-sampling
Good for coarse and firm
bottom sediments
Adequate for most substrates that are not compacted

Deep lakes,
rivers, and
estuaries; useful
on sand, silt, or
clay

Chapter 5 Aquatic Sediment Sampling

May not penetrate sediment to desired depth,


especially in consolidated
sediments
Susceptible to incomplete
closure and loss of
sample
Requires more casts to
obtain sufficient sample if
many analyses needed

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Sample
Depth
(cm)

Sample
Volume
(L3)

0 30

18 75

Adequate on most substrates May not close completethat are not compacted
ly, resulting in sample
Large sample obtained
loss
May close prematurely in
intact, permitting subrough waters
sampling
Available in stainless steel Metal frame may contaminate sample
Heavy, requires winch

Modified
Lakes and
Van Veen (e.g., marine areas
Ted Young
Grab)

0 15

18.0

Petersen

0 30

9.45

Fluorocarbon plastic liner


Requires winch
can help avoid metal conta- Relatively expensive
mination
Screened bucket cover helps
reduce bow wave effects
Provides large sample
Shock wave from descent
Penetrates most substrates
may disturb fine-grained
sediment
Lacks lid cover to permit
sub-sampling
May not close completely,
resulting in sample loss
Metal frame may contaminate sample
Restricted to low current
conditions
May exceed target penetration depth

Shipek, standard Used primarily in


marine waters
and large, inland
lakes and reservoirs; not useful
for compacted
sandy clay or till
substrates

0 10

3.0

Sample bucket opens to


permit sub-sampling
Retains fine-grained sediments effectively

Metal frame may contaminate sample


Heavy, requires winch
Can result in loss of the
topmost 23 cm of very
fine, unconsolidated sediment

Shipek, mini

03

0.5

Handles easily without


winch or crane from most
platforms

Requires vertical penetration


Samples small volume
May lose fine-grained
sediment
May close prematurely

Device
Van Veen

Use
Deep lakes,
rivers, and
estuaries; useful
on sand, silt, or
clay; effective in
marine environments in deep
water and strong
currents

Deep lakes,
rivers, and
estuaries; useful
on most substrates

Lakes, useful for


most substrates
that are soft

Chapter 5 Aquatic Sediment Sampling

Advantages

Disadvantages

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Table 5-4. Advantages and Disadvantages of Commonly Used Core Samplers


(For illustrations of specific coring equipment, see http://clu-in.org/programs/21m2/sediment/)
Device/
Dimensions

Use

Sample
Depth
(cm)

Sample
Volume (L3)

Advantages

Disadvantages

Fluorocarbon
plastic or glass
tube (3.5 7.5 cm
inner diameter
(I.D.); 120 cm
long)

Shallow wadeable waters or


deep waters if
SCUBA
available; soft
or semiconsolidated
deposits

0 10

0.096 0.44 Preserves layering and


Small sample size necessipermits historical study of
tates repetitive sampling
sediment deposition
Minimal risk of contamination
Rapid; samples immediately
ready for laboratory shipment

Hand corer with


removable fluorocarbon plastic or
glass liners (3.5
7.5 cm I.D.; 120
cm long

Same as above
except more
consolidated
sediments can
be obtained

0 10

0.96 0.44

Same advantages as fluorocarbon plastic or glass tube


Penetrates substrate with
greater ease through use of
handles

Small sample size necessitates repetitive sampling


Requires careful handling
to prevent spillage
Requires removal of liners
before repetitive sampling
Barrel and core cutter
metal may contaminate
sample

Box corer

Same as above
but the depth of
the unconsolidated
sediment must
be at least 1 m

0 70

30.0

Collects large, undisturbed


sample; optimal for obtaining intact subsamples

Difficult to handle
Relatively heavy, requiring larger vessel and power winch to deploy

Gravity corer,
Phlegar Corer (3.5
cm I.D., 50 cm
long)

Deep lakes and


rivers; semiconsolidated
sediments

0 50

0.48

Reduces risk of sample


Requires careful handling
contamination
to avoid sediment spillage
Maintains sediment integrity Requires repetitive and
relatively well
time-consuming operation
Penetrates with sharp cutting
and removal of liners due
edge
to small sample size

Gravity corer,
Kajak-Brinkhurst
Corer (5 cm I.D.,
70 cm long)

Deep lakes and


rivers; soft finegrained sediments

0 70

1.37

Collects greater volume than Same as Phlegar Corer


the Phlegar Corer

03m

10.26

Retains complete sample


from tube because the core
valve is fitted to the core
liner
Fins promote vertical penetration

Benthos gravity
Soft, finecorer (6.6, 7.1 cm grained sediI.D., 3 m long)
ments

Chapter 5 Aquatic Sediment Sampling

Requires weights for deep


penetration so the required
lifting capacity is 750
1,000 kg
Requires vertical penetration
Compacts sediment sample

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Device/
Dimensions

Use

Alpine gravity
Soft, finecorer (3.5 cm I.D.) grained semiconsolidated
substrates

Piston corers

Ocean floor and


large deep
lakes; most
substrates

BMH-53 piston
corer

Waters 2 m
deep with
extension rod;
soft deposits

Boomerang corer
(6.7 cm I.D.)

Ocean floor (up


to 9,000 m
deep)

Vibracorer
Continental
(5.0 7.5 cm I.D.) shelf of oceans,
large lakes;
sand, silty sand,
gravelly sand
substrates

Sample
Depth
(cm)

Sample
Volume (L3)

2m

Advantages

Disadvantages

1.92

Allows different penetration


depths due to interchangeable steel barrel

Lacks stabilizing fins for


vertical penetration
May penetrate nonvertically and incompletely
Requires a lifting capacity
of 2,000 kg
Disturbs sediment stratas
and integrity
Compacts sediment sample

3 20 m

5 40

Typically recovers a relative- Requires lifting capacity


ly undisturbed sediment core
of 2,000 kg
in deep waters
Piston and piston positioning at penetration may fail
Disturbs surface
(0 0.5 m)

2m

Piston provides for greater


sample retention

Cores must be extruded


onsite to other containers
Metal barrels introduce
risk of metal contamination

1m

3.52

Requires minimal shipboard


equipment so small vessels
can be used

Only penetrates 1.2 m


Requires calm water for
recovery
Loses 10 20% of sample

36m

Chapter 5 Aquatic Sediment Sampling

5.89 13.25 For deep profiles it effectively samples most substrates


with minimum disturbance
Can be used in over 20 m of
water depth
Portable models can be
operated from small vessels
(e.g., 10 m long)

Labor intensive
Assembly and disassembly
might require divers
Disturbs surface
(0 0.5 m) layer
Special generator may be
needed
Heavier models require
larger boat and power
winch to deploy

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Table 5-5. A Summary of Stream Net Samplers Used to Collect Organisms from Flowing Water
Net Sampler

Habitats and
Substrates

Effectiveness of
Device

Advantages

Limitations

Surber Stream
Bottom Sampler

Shallow, flowing
streams, less than
32 cm in depth
with good current;
rubble substrate,
mud, sand, and
gravel

Performance
depends on
current and
substrate

Encloses area
sampled; easily
transported or
constructed; samples a unit area

Difficult to set in
some substrate
types, that is large
rubble; cannot be
used efficiently in
still, slow-moving
streams

Portable Invertebrate Box Sampler

Same as Surber

Same as Surber

Same as Surber
except completely
enclosed with
stable platform; can
be used in weed
beds

Same as Surber

Hess Sampler

Same as Surber

Same as Surber

Same as Surber
except completely
enclosed with
stable platform; can
be used in weed
beds

Same as Surber

Hess Stream
Bottom Sampler

Same as Surber

Same as Surber

Same as Surber
except completely
enclosed with
stable platform; can
be used in weed
beds

Same as Surber

Stream-bed Fauna
Sampler

Same as Surber

Same as Surber

Same as Surber
except completely
enclosed with
stable platform; can
be used in weed
beds

Same as Surber

Drift Nets

Flowing rivers
and streams; all
substrate types

Effective in
collecting all
taxa which drift
in the water
column

Low sampling
error; less time,
money, and effort;
collects macroinvertebrates from all
substrates; usually
collects more taxa

Unknown where
organisms come
from; terrestrial
species may make
up a large part of a
sample in summer
and periods of wind
and rain; does not
collect non-drifting
organisms

Chapter 5 Aquatic Sediment Sampling

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For separating biota from sediment, standardized


sampling techniques (both collection and sieve
mesh size) should be followed. The use of different sieve mesh sizes for screening benthic samples limits the comparability of results between
marine monitoring studies. A major advantage of
using a smaller mesh size is the retention of both
juvenile and adult organisms as well as large-and
small-bodied taxa; however, a disadvantage is the
increased time and cost of sample processing.
On-board the vessel, sieving typically occurs
prior to sample preservation. If it is necessary to
hold samples for later sieving, preservation
proceeds sieving. When sub-sampling (subcoring within a grab or core sample) is necessary,
issues related to sub-sampling include representativeness (some benthic species have patchy distributions); and possibly damage to organisms
such as worms, thereby diminishing the number
of specimens that can be identified. All organisms found within the sub-core should be counted
and identified.
5.8.1. Benthic Habitat Mapping
Benthic habitat mapping provides a method for
relating source and distributions of contaminated
sediments to sensitive or valuable aquatic resources and overall benthic habitat quality. Benthic surveys require the use of physical and biological sampling techniques. Large study areas
require wide area assessments with remote sensing via hydrographic and sonar surveys to determine the physical characteristics of the benthic
site without disturbing the bottom. Differing
topography, sediment, and vegetation types may
be resolved from sound and light reflectance
patterns. Ground-truthing with finer-scale sampling methods should be used to validate interpretations of the remote-sensing data.
No single mapping method provides a comprehensive picture, so the ability to integrate, analyze, and interpret several different types of data
is required in order to conduct a field-scale ecological risk assessment. Regardless of which
methods are used, benthic data must be analyzed
and interpreted for use in benthic habitat mapping. The analysis tools include GIS, habitat
spatial analysis, and statistical or visual evaluaChapter 5 Aquatic Sediment Sampling

tion of benthic data and contaminant concentrations. The benthic habitat may need to be monitored over time to determine the effects of habitat
change due to natural or human impacts, and to
assure effective implementation of remediation
strategies.
5.8.2.

Toxicity Testing in Microcosms or


Mesocosms
Toxicity testing of benthic macroinvertebrates,
discussed briefly in Section 5.6, can complement
the sediment quality and associated risk. Standard toxicity practices usually involve laboratory
or field exposure chambers where organisms are
exposed to natural or elevated contaminant concentration levels to assess acute and chronic risks.
Attempts to obtain field data for risk assessment
of contaminants released into marine/estuarine
systems are often complicated by a number of
factors such as complex circulation and mixing
patterns, stratification, dynamic, short-term
changes as well as seasonal movements of biota,
and the ecosystems physical scale.
In recent years, microcosm and mesocosm testing
has gained wide acceptance for ecological risk
assessment. Microcosms and mesocosms are
simulated ecosystems containing water, sediment,
and communities of plants and invertebrates from
field sites to be established in laboratory aquaria
or in designed field systems using enclosures or
caissons. Temperature, rainfall, sunlight, sediment disturbance, water circulation, bioturbation,
and other natural processes can affect chemical
behaviors, making it difficult to determine precisely the fate and effects of contaminants within
a complex ecosystem. These simulated systems
permit environmental variables to be controlled in
a manner that cannot be achieved in field studies.
Simulated systems may be used to evaluate higher-level ecological effects of chemicals on populations and communities. They also allow monitoring of biodegradation, natural attenuation,
biota population and habitat recovery, and bioremediation.
Tests conducted in simulated ecosystems are
subject to constraints that restrict the effect of
physical forces, limit physical scale of the test,
and introduce biases from chemical partitioning
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and processing along the walls of the test system.


These constraints should be considered in the
evaluation, but the simulated ecosystem approach
still has broad application as a model of dynamic
marine systems.
Mesocosms are large-scale systems that allow
investigators to study and collect data over a large
area. These systems are usually outdoor systems
such as ponds or enclosures within a larger body
of water, typically a lake, river, marsh, or ocean.
For sediment ecological risk assessment purposes, the microcosm approach generally allows
more efficient data collection.
Microcosm testing results are considered by most
regulatory authorities to be more representative of
natural conditions than results of conventional
toxicity tests, which justifies the use of a smaller
safety factor. For example, many aquatic populations and communities tolerate chemical exposures higher than the 50 percent lethal concentration (LC50), and even sensitive test species tolerate exposures greater than the no-effect concentration (NOEC), due to factors such as population
recovery or succession, water dilution, sediment
transport, and other environmental factors. Microcosm results may be used to justify a higher
effects threshold in these cases. Extended benthic
toxicity studies can be used to justify a more
accurate and less conservative assessment of
ecological risk. Many regulatory authorities
acknowledge that effects to the benthic community are not ecologically significant should the
population recovery occur within a reasonable
period of time, typically a growing season. Mirocosms have been used to demonstrate recovery in
the following ways:

observed in the field when chemicals disappear


due to degradation or water movement
Periodic reintroduction of invertebrates or
algal organisms, which simulates natural immigration and allows observation of population
recovery
Simulation of conditions during which chemical concentrations in the water decrease over
time, which may demonstrate recovery of invertebrate populations
Benthic colonization by invertebrate species
and populations may be evaluated by transferring contaminated field sediments in open tray
containers to uncontaminated or reference field
sites, where they are periodically monitored.
Benthic colonization and recruitment from the
water column may be measured by invertebrate community indices (species, abundance,
diversity, evenness, dominance, richness).
Benthic colonization may also be investigated
by transferring contaminated sediments from
the field to a flow-though, unfiltered laboratory
seawater system where observations and measurements can be made more frequently.
For more information on benthic macroinvertebrate investigations, consult the following references:

Addition of spiked sediments to field sediments allows chemicals to partition between


water and sediment as they would do in a natural environment; a water-sediment system may
reduce toxicity by sorption which reduces the
bioavailability of the compound in the watersediment system compared to a water-only
system
Variation of chemical concentrations over
time, to simulate exposure patterns typically

Chapter 5 Aquatic Sediment Sampling

Standard Test Method for Measuring the


Toxicity of Sediment-Associated Contaminants with Estuarine and Marine Invertebrates
(Ref. 20)
Standard Test Method for Measuring the
Toxicity of Sediment-Associated Contaminants with Freshwater Invertebrates (Ref. 24)
Standard Guide for Conducting Sediment
Toxicity Tests with Polychaetous Annelids
(Ref. 25)
Estuarine and Coastal Marine Waters Bioassessment and Biocriteria Technical Guidance
(Ref. 26)
Environmental Monitoring and Assessment
Program Surface Waters: Field Operations
and Methods for Measuring the Ecological
Condition of Wadeable Streams (Ref. 27)
Rapid Bioassessment Protocols for Use in
Streams and Wadeable Rivers: Periphyton,
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Benthic Macroinvertebrates and Fish (Ref.


28)
Methods for Measuring the Toxicity and
Bioaccumulation of Sediment-associated
Contaminants with Freshwater Invertebrates Second Edition (Ref. 29)
Methods for Assessing the Chronic Toxicity
of Marine and Estuarine Sediment-associated
Contaminants with the Amphipod Leptocheirus Plumulosus (Ref. 30)
Comparisons of Boating and Wading Methods Used to Assess the Status of Flowing
Waters (Ref. 31)
Logistics of Ecological Sampling on Large
Rivers (Ref. 32).

Chapter 5 Aquatic Sediment Sampling

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5.9. References
1

EPA-823-F-01-023, Methods for Collection, Storage and Manipulation of Sediments for


Chemical and Toxicological Analyses: Technical Manual
(http://water.epa.gov/polwaste/sediments/cs/upload/factsheet.pdf)

EPA-905-B02-001-A, A Guidance Manual to Support the Assessment of Contaminated


Sediments in Freshwater Ecosystems. Volume I - An Ecosystem-Based Framework for Assessing and Managing Contaminated Sediments
(http://www.epa.gov/glnpo/sediment/Vol1.pdf)

EPA-540-R-05-012, Contaminated Sediment Remediation Guidance for Hazardous Waste


Sites (http://www.epa.gov/superfund/health/conmedia/sediment/pdfs/guidance.pdf)

NFESC UG-2053-ENV, Implementation Guide for Assessing and Managing Contaminated


Sediment at Navy Facilities
(http://web.ead.anl.gov/ecorisk/related/documents/rev_fin_Imple_Guide_for_Sediment_1.pd
f)

MESO-02-TM-01, Critical Issues for Contaminated Sediment Management


(http://www.clu-in.org/download/contaminantfocus/sediments/critical-sediment-mgtsedmgt.pdf)

Measurement and Monitoring Technologies for the 21st Century, Sampling for Contaminants
In Sediments and Sediment Pore Water (http://clu-in.org/programs/21m2/sediment/)

EPA Handbook, A Compendium of Chemical, Physical and Biological Methods for Assessing and Monitoring the Remediation of Contaminated Sediment Sites
(http://www.epa.gov/eerd/methods/108Complete.pdf)

EPA-503/8-91/001, Evaluation of Dredged Material Proposed for Ocean Disposal Testing


Manual http://water.epa.gov/type/oceb/oceandumping/dredgedmaterial/upload/gbook.pdf

EPA-823-B-98-004,Evaluation of Dredged Material Proposed for Discharge in Waters of


the U.S- Testing Manual, Inland Testing Manual.
http://www.spn.usace.army.mil/conops/References/National_Guidance/ITM-OTM-UTMFramewk/ITM/%20ITM.pdf

10

NFESC UG-2041-ENV, Guide for Incorporating Bioavailability Adjustments into Human


Health and Ecological Risk Assessments at U.S. Navy and Marine Corps Facilities
(http://aec.army.mil/usaec/cleanup/bioavailability01.pdf)

11

ITRC 2011, Incorporating Bioavailability Considerations into the Evaluation and Remediation of Contaminated Sediment Sites (http://www.itrcweb.org/contseds-bioavailability)

12

EPA-905-B94-002, Assessment and Remediation of Contaminated Sediments (ARCS) Program - Assessment Guidance (http://www.epa.gov/glnpo/arcs/EPA-905-B94-002/EPA-905B94-002.html)

13

ASTM E1391, Standard Guide for Storage, Characterization, and Manipulation of Sediments for Toxicological Testing and for Selection of Samplers Used to Collect Benthic Invertebrates

14

ASTM D4687, Standard Guide for General Planning of Waste Sampling

Chapter 6 Aquatic Sediment Sampling

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15

ASTM D4823, Standard Guide for Core Sampling Submerged, Unconsolidated Sediments

16

ASTM D4387, Standard Guide for Selecting Grab Sampling Devices for Collecting Benthic
Macroinvertebrates

17

Mudroch, A. and S. MacKnight, (Eds). 1994. Handbook of Techniques for Aquatic Sediments Sampling, Second Edition, Lewis Publishers, Boca Raton, FL.

18

Mudroch, A. and J. Azcue, 1995. Manual of Aquatic Sediment Sampling. Lewis Publishers,
Boca Raton, FL.

19

ASTM D3976, Standard Practice for Preparation of Sediment Samples for Chemical Analysis

20

ASTM E1367, Standard Test Method for Measuring the Toxicity of Sediment-Associated
Contaminants with Estuarine and Marine Invertebrates

21

ASTM E729, Standard Guide for Conducting Acute Toxicity Tests on Test Materials with
Fishes, Macroinvertebrates, and Amphibians

22

NFESC Technical Report 1902, Coastal Contaminant Migration Monitoring: The Trident
Probe and UltraSeep System: Hardware Description, Protocols, and Procedure
(http://www.spawar.navy.mil/sti/publications/pubs/tr/1902/tr1902cond.pdf)

23

NFESC Technical Report 1966, Monitoring of Water and Contaminant Migration at the
GroundwaterSurface Water Interface
(http://www.spawar.navy.mil/sti/publications/pubs/tr/1966/tr1966cond.pdf)

24

ASTM E1706, Standard Test Method for Measuring the Toxicity of Sediment-Associated
Contaminants with Freshwater Invertebrates

25

ASTM E1611, Standard Guide for Conducting Sediment Toxicity Tests with Polychaetous
Annelids

26

EPA-822-B-00-024, Estuarine and Coastal Marine Waters Bioassessment and Biocriteria


Technical Guidance
(http://water.epa.gov/scitech/swguidance/standards/criteria/aqlife/biocriteria/upload/2009_04
_22_biocriteria_States_estuaries_estuaries.pdf)

27

EPA/620/R-94/004F, Environmental Monitoring and Assessment Program Surface Waters:


Field Operations and Methods for Measuring the Ecological Condition of Wadeable Streams
(http://www.epa.gov/emap/html/pubs/docs/groupdocs/surfwatr/field/ws_abs.html)

28

EPA-841-B-99-002, Rapid Bioassessment Protocols for Use in Streams and Wadeable Rivers: Periphyton, Benthic Macroinvertebrates and Fish - Second Edition
(http://water.epa.gov/scitech/monitoring/rsl/bioassessment/index.cfm)

29

EPA/R-99/064, Methods for Measuring the Toxicity and Bioaccumulation of Sedimentassociated Contaminants with Freshwater Invertebrates - Second Edition
(http://water.epa.gov/polwaste/sediments/cs/upload/freshmanual.pdf)

30

EPA/600/R-01/020, Methods for Assessing the Chronic Toxicity of Marine and Estuarine
Sediment-associated Contaminants with the Amphipod Leptocheirus Plumulosus
(https://www.clu-in.org/download/contaminantfocus/sediments/leptocheirusj.pdf)

31

EPA/600/R-01/108, Comparisons of Boating and Wading Methods Used to Assess the Status
of Flowing Waters (http://www.epa.gov/eerd//methods/MCD_nocover.pdf)

Chapter 5 Aquatic Sediment Sampling

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32

EPA/600/R-00/109, Logistics of Ecological Sampling on Large Rivers


(http://www.epa.gov/eerd/methods/logistics_nocover.pdf)

Chapter 5 Aquatic Sediment Sampling

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Chapter 6. Surface Water Sampling


6.1. Purpose
This chapter provides general guidelines and
procedures for sampling approaches, methods,
and equipment used for surface water sampling.
Following these guidelines and procedures will
greatly enhance the representativeness of the
samples and accurately characterize source conditions. This chapter will help project planning and
sampling personnel to evaluate available information on a sampling location, select an appropriate
sampling approach, select and utilize sampling
equipment, and incorporate appropriate QA/QC
samples.
6.2. Scope
Surface waters are water bodies that rest or flow
over land, with a surface that is open to the atmosphere. Surface water samples are collected
from streams, rivers, lakes, ponds, creeks, lagoons, estuaries, surface impoundments, or coastal waters. Samples can be collected at the surface
level of the subject water body or at a prescribed
depth interval. Samples can be analyzed to characterize surface water quality or determine pollutant concentrations.
The procedures presented in this chapter are
typical and can be modified as required to accommodate site conditions and equipment or
procedural limitations. Field sampling should be
conducted in accordance with appropriate federal,
state, or local government compliance requirements and guidelines.
6.3. Project Planning
This section provides an overview of the planning
process for conducting a surface water sampling
program. Included in this section is a discussion
of sampling strategy, development of a sitespecific SAP, and QA considerations.
Before a surface water sampling program can
begin, concise objectives should be developed
regarding the intent of the sampling program.
The objectives provide the framework for developing a sampling strategy for the site and preparing the SAP.
Chapter 6 Surface Water Sampling

6.3.1. Sampling Strategy


The sampling strategy is designed around the
objectives and begins with a review of the CSM.
Refer to Chapter 2 for more information on CSM
development. This model will help the Project
Manager determine whether samples should be
collected at the surface level or at a depth interval. The model also will help to determine
whether a sample should be collected at a single
location and point in time, or whether multiple
samples should be collected over time, locations,
or depth intervals and combined into a representative sample for analysis. From this information,
the Project Manager can establish appropriate
sampling locations, number and type of samples
required, and an appropriate type of sampling
equipment for the site conditions.
6.3.2. Site-Specific SAP
The goal of a surface water sampling program is
to collect a representative sample of the current
surface water conditions. The development of a
site-specific SAP is the first step toward collecting a representative surface water sample. Each
SAP is an instruction manual for field personnel.
It should be built around the objectives and sampling strategy. See Chapter 2 of this handbook
for a detailed discussion of SAP development
applicable to all sampling programs.
The SAP should consider a variety of factors,
including site hydrogeology, the condition and
accessibility of sampling locations, suspected
pollutants, DQOs, analytical methods, detection
limits, surface water collection methods, sample
handling procedures, and safety precautions.
The SAP cannot be implemented effectively if
field personnel do not understand its contents.
Many times, the primary reason that surface
water sampling events are problematic is that the
person preparing the SAP is not the person in the
field. One method that alleviates this problem is
assigning a Sampling Team Leader who is responsible for all activities in the field. The Sampling Team Leader has the appropriate level of
training and experience, and will work closely
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with those individuals preparing the SAP to


understand fully the objectives of the program.
The Sampling Team Leader is responsible for all
individuals in the field. If required, he or she also
is responsible for providing additional training to
field personnel before fieldwork begins.
6.3.3. QA
The level of data quality for each surface water
sampling program, and many times for each
specific sampling event, depends on the intended
use of the data. It is important to remember,
regardless of the level of QA/QC for any surface
water sampling program, that sample integrity
must be maintained during sample collection.
Laboratory analysis, no matter how sophisticated,
is representative only if the sample supplied to
the analyst has retained its integrity.
To determine the level of quality required for
each surface water sampling program or event,
Site Managers and those responsible for data
integrity should begin with a systematic planning
process that helps define the DQOs. The DQOs
clarify the study objectives, define the most
appropriate type of data to collect, determine the
most appropriate conditions for data collection,
and specify tolerable error limits on decisions that
will be used as the basis for establishing the
quantity and quality of data needed to support the
decision. See Chapter 2 of this manual for detailed information on QA/QC, including the
systematic planning process, development of
DQOs, and preparation of SAPs.
The following protocol should be used to ensure
integrity and accuracy of the data collected during
surface water sampling:

The laboratory analysis should be performed


by an appropriately certified or accredited
laboratory for the required methodology
All samples must be accompanied by a
completed COC record
The field blank, trip blank, equipment blank,
and field duplicate samples should be
collected, as appropriate, to provide for data
evaluation to determine the accuracy and
representativeness of surface water samples

Chapter 6 Surface Water Sampling

The field decontamination process must be


followed properly to ensure QC of the field
sampling
MS/MSDs should be performed by the
laboratory at a rate of one set per analyte,
matrix, and preparation batch of up to a
maximum of 20 samples, to validate the
method selected with the matrix being
analyzed
The specific frequency of QC sample
collection should be specified in the SAP,
which is discussed in Chapter 2 and Appendix
C.
Final data should be reviewed for correctness of
numerical input, equation selection, and numerical calculations. Each site QA/QC varies with the
degree of contamination, regulatory requirements,
and site location.
6.4. Hazards and Safety Precautions
A site-specific HASP that addresses all anticipated hazards for each task should be prepared.
The following discussion addresses common
hazards associated with surface water sampling
activities. Refer to Chapter 2 of this handbook
for specific hazard identification techniques and
detailed control methods.
When sampling surface impoundments, appropriate precautions must be employed to ensure the
safety of sampling personnel. The sampling team
member collecting the sample should not get too
close to the edge of the impoundment, where
bank failure may cause the sampler to lose his
balance. The person performing the sampling
should be on a lifeline and wear appropriate PPE.
When performing sampling from a boat in an
impoundment or flowing waters, follow appropriate boating safety procedures. In any situation
where a body of water being sampled is deeper
than two feet, the sampling team should wear
coast guard-approved life vests.
If the surface impoundment contains known or
suspected hazardous substances, the need to
collect samples versus the potential risk to sampling personnel must be considered. If sampling
is determined to be necessary, appropriate protective measures (e.g., use of a flat-bottomed boat
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for increased stability, life vests and preservers,


and a back-up team) must be implemented.
When working with potentially hazardous materials, follow appropriate OSHA health and safety
procedures.
6.5. Field Preparation
Surface water samples are collected from different types of water bodies with variable site conditions. Regardless of the water source, the following tasks should be completed prior to any sampling event:

Determine the extent of the sampling effort,


the sampling methods to be employed, and the
types and amounts of equipment and supplies
needed
Obtain the necessary sampling and monitoring
equipment, decontaminate or pre-clean the
equipment, and ensure that it is in working order
Prepare scheduling, and coordinate with staff,
clients, and regulatory agencies, if appropriate
Perform a general site survey prior to site
entry, in accordance with the site-specific
HASP
Use stakes, flags, buoys, or portable GPS
coordinates to identify and mark all sampling
locations. If required, the proposed locations
may be adjusted based on site access, property
boundaries, and surface obstructions. If collecting sediment samples, this procedure may
disturb the bottom, resulting in the suspension
of fine sediment particulates into the water
column. To avoid sediment disturbance, river
or stream sampling should start from downstream location toward upstream location.

6.5.1.

Representative Sampling
Considerations
To collect a representative sample, the hydrology,
shape, and size of an impoundment should be
determined prior to sampling. This will aid in
determining the presence of phases or layers in
lagoons, flow patterns in streams, and appropriate
sample locations and depths.

Chapter 6 Surface Water Sampling

A preliminary surface water quality survey


should measure pH, temperature, and DO at
points along shorelines, wetlands, creeks, and
ponds. Measurements should be collected at
1meter intervals from the substrate to the surface
using the appropriate monitoring instruments.
For shallow waters, measurements should be
taken within the top 12 inches of the water column. Measurements of pH, temperature, DO,
conductivity, and oxidation-reduction potential
can assist in the interpretation of analytical data
and the selection of sampling sites and surface
water sample collection depths.
Consider the following factors when selecting a
sampling device for collecting surface waters:

Will the sample be collected from shore or


from a boat?
At what depth should the sample be collected?
What is the overall depth and flow direction of
the river or stream?
What type of sample will be collected (e.g.,
water or lagoon liquids)?
For contamination of surface water from a point
source, such as an outfall or sewer line, sampling
may be based on visual evidence of seepage or
discharge streams. Sampling points should be
established at the locations where distinct
changes in pH, temperature, DO, or conductivity
indicate the possible presence of contamination or
leachate discharge. A GPS unit may be used to
determine the coordinates of the sampling location in terms of latitude and longitude. Field
equipment that should be available at the time of
sampling is listed in Section 6.7.
Prior to sampling at each location, record the
following information in the FLB/FN:

Sample location, ID number, date, and water


temperature at the time of collection
pH, DO, conductivity, and depth of water (if
applicable) at the sample collection location,
along with any equipment calibration data
Water depth at the midpoint or center of the
water body, if applicable

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Description of site and weather conditions at


time of sampling, as well as the physical
characteristics of the sample.

and precautions when developing a representative


sampling design, which include:

6.5.2. Point Source Investigations


A contaminant in a discharge that feeds into a
water body at a discernible, confined, and discrete
conveyance is defined as a point source pollutant.
An example of a point source discharge is effluent from a storm water sewer into a river through
a pipe, ditch, or tunnel. Point sources are regulated under the CWA and NPDES, through permit application and approval. Sampling of these
sources may be performed for characterizing
discharges for permit application, with the collected data serving as a basis for establishing
permit requirements for monitoring and reporting.
Monitoring and analytical requirements are established by permit on a site-specific basis.
Storm water and other effluent samples that feed
into a surface water body should be collected at
the point source. To ensure that representative
point source samples are collected in storm water
investigations, specific criteria for the type of
storm event that is sampled have been established. Criteria recommended by the EPA for
NPDES sampling include the depth of the storm
must be greater than 0.1 inch of accumulation, the
storm must be preceded by at least 72 hours of
dry weather, and the depth of rain and duration of
event should not vary by more than 50 percent
from the average depth and duration. These
criteria ensure that adequate flow will be discharged, allow for build-up of pollutants during a
dry interval, and ensure that the storm would be
representative. State requirements may differ.
6.5.3. Nonpoint Source Investigations
A pollutant that feeds into a water body from a
source that cannot be traced back to a single
origin, such as storm water runoff, is termed a
nonpoint source pollutant. These pollutants are
monitored to determine impacts on the water
quality of rivers, streams, and bays for compliance with state and local management plans.
When sampling for a nonpoint source investigation, it is important to consider special properties

Chapter 6 Surface Water Sampling

Stratification. Water body stratification


occurs as a result of temperature or thermal
conditions. Water temperature profile controls
circulation in the water body. Warmer, less
dense surface water and colder, deeper water
become stratified with rapid variance of
temperature and increasing depth intervals.
Chemically induced stratification results when
levels of a water body are separated by a steep
salinity gradient. Still-water bodies, such as
lakes and reservoirs, have a greater tendency
to stratify than rivers or streams. One layer or
zone of the water body may be exposed to a
discharge point, the atmosphere, or another
pathway of contamination, which can yield
characteristics that are different from other
layers or zones in the water body.
Current. The movement, or current, in a
water body can disturb mixing zones and
reduce the chances of obtaining a representative sample
Storm Events. Storms may turn over strata in
a water body and reduce the representativeness
of a sample. Precipitation or runoff may
increase or reduce representative
concentrations of contaminants of interest.
Time of Year. Temperate water bodies
experience overturn during the fall and spring
season. As the air temperature warms or cools
with the start of the new season, conditions in
the lake change from stratified to isothermal,
causing the entire water body to mix and
overturn, until stratification is re-established.
Time of year also influences rainy and dry
periods, which affect total volume and
velocity.
Circulation. Movement in a water body may
be the result of wind action or water density
gradients. Sediment distribution may be
dominated by water motion.
Velocity. The speed at which a surface water
body flows affects the selection of sampling
locations, times, equipment, and techniques.
When sampling at a river bend, velocity is the

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greatest where the radius is smallest (i.e.,


towards the inside bank).
Turbidity. Surface water can contain
contaminants that adhere to the particles of
suspended solids or fine particulates of
sediment. These suspended sediments adhere
to the water surface and will add to the water
sample. Turbidity will vary due to mixing and
settling in the water body.
Salinity. The natural salt concentration, or
salinity, of a water body may vary with
proximity to the ocean, seasonal gradients, and
stratification. Tidal phases of the water body
must also be considered when sampling in
saline waters.
For water quality investigations, surface water
runoff samples should be collected at upstream
and downstream locations on a subject water
body. In areas where tidal influence is a consideration, a timed composite sample should be
taken, with care to avoid cross-contaminating the
samples. The composite sampling procedure
must be based on the DQOs for data interpretation and assessment. Identify specific sampling
locations and procedures in the SAP.
Additional sampling locations might be considered, depending upon the size of the site, the
number of streams or rivers near the site, and the
location of natural drainage swales and wetlands.
If contamination of a river is suspected or documented, river or sea water levels and corresponding flow should be monitored upstream
from the site and downstream from any leachate
seeps or runoff. This information can be used to
assess dilution effects and potential seasonal
variations in contaminant concentrations due to
changing water levels.
Often, the U.S. Geological Survey (USGS), state
agencies, and public water supplies monitor river
and stream flow and water quality at various
points along major rivers or streams. Resulting
data are publicly available and can be used for
determining water levels, flow rates, and drainage
and water quality information. Precipitation data
can be acquired from local weather bureaus or the
National Climatic Data Center in Asheville,
North Carolina.
Chapter 6 Surface Water Sampling

Nonpoint sources may feed into intermittent


streams. These streams often transport contamination from a site because of surface water runoff
during or after a period of heavy rainfall. If
contamination is suspected because of seasonal
runoff, surface water samples should be collected
during and/or immediately following periods of
heavy rainfall.
For investigations of compliance with storm
water permit, an evaluation of the optimal sampling locations should be made. The EPA storm
water program provides guidance for selecting
potential sampling locations and determining the
concentration of contaminants during rainfall
events. It is particularly important to sample the
storm flow runoff from the first 30 minutes of
significant flow if not otherwise specified in the
storm water permit. One sample should be collected where runoff or overflow enters the stream
as well as other locations upstream of the site.
Intermittent streams are not usually monitored by
other agencies, so the stream depth, width, and
flow rate during or after periods of heavy rainfall
should be measured. The USGS can be consulted
for an estimation of water drainage in particular
areas.
Storm water permits often require the collection of
one grab sample of constant volume, not less than
100 milliliters, every 20 minutes during the storm
event, over a period of at least 3 hours. These grab
samples are combined into a composite sample for
analysis. Refer to Section 6.6 for more information on grab samples and composite samples. As
an alternative to a time-weighted sample, a flowweighted sample may be taken in which the volume of each grab sample to be composited is
proportional to the flow rate of the discharge at the
time the sample was collected.
6.5.4. Leachate
In most cases, a leachate well is installed as part
of a remedial action or site characterization.
Leachate wells are monitored following groundwater sampling procedures as defined in the
operating permit of the facility or site.
Leachate sample collection locations should
include the outfalls to shorelines. The location of
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leachate discharge ultimately depends on the


sites physical and geological characteristics.
Leachate can move laterally below ground toward
a creek or stream to affect surface water quality.
Samples should be collected both upstream and
downstream of the site to determine the extent of
contamination. In some cases, the leachate can
outcrop at the top and the side of the site and flow
with the surface water body. Samples should be
collected not only at the leachate seeps but also
upstream of them.
At each seep location, the sampler should collect
samples by immersing the sample container
directly in the seep. If the depth of water in the
seep is not sufficient to submerge the sample
container, then use a dedicated pre-cleaned container to collect the sample.
For any sample collection method used, more
than one round of sampling is recommended for
characterization of leachate. A minimum of two
sampling events, one during a dry period and
another during or immediately after precipitation,
should be performed to determine variability in
leachate composition. The collected samples are
analyzed for any combination of the following
parameters: priority pollutant organics, metals,
cyanide, biochemical oxygen demand (BOD),
chemical oxygen demand (COD), pH, total dissolved solids (TDS), total suspended solids
(TSS), oil and grease, TOC, chloride, nitrate,
phosphate, ammonia, and sulfide. All samples
should be analyzed according to the permit requirements.
6.5.5. Wetland Sampling
Contaminant sources may exist around natural
wetlands or other sensitive environments. Contamination from these sources can migrate from
the site through surface water into wetlands,
which can adsorb heavy metals and complex
organics, affecting the health of the wetlands.
Wetlands are defined in accordance with the
Federal Manual for Identifying and Delineating
Jurisdictional Wetlands (U.S. Fish and Wildlife
Service et al., 1989).
Wetlands sampling for chemical and biota studies
may be performed as part of permit applications.
Chapter 6 Surface Water Sampling

Composite or grab samples of surface water or


sediment may be collected as described in the
permit or defined in the SAP. The SAP will
describe the procedures to meet the DQOs for
interpreting the environmental impact of suspected contamination. When sampling in a designated wetland, it is vital to minimize the impact
of the sampling event on the environment.
6.6. Sampling Procedures
Prior to initiating any field sampling activity,
sampling personnel should review the HASP. All
monitoring instruments and PPE should be
checked thoroughly at this time. Prior to sampling at each location, water monitoring equipment probes should be decontaminated using
procedures appropriate for the contaminant
present and then rinsed thoroughly with ASTM
Type II or better quality water.
Surface water sampling includes the collection of
samples from lakes, ponds, streams, and rivers. It
may be necessary to collect liquid samples from
lagoons, surface impoundment, sewers, and
leachate seeps. Actual sampling situations encountered in the field may vary according to the
site. The most important goal of surface water
sampling is to collect a representative sample of
the appropriate horizons or phases present in the
liquid.
Surface water can be collected either as a grab or
as a composite sample. A grab sample is an
individual sample collected randomly at a specific time element. A composite sample is a representative sample prepared from a combination of
multiple grab sample aliquots collected at periodic time intervals or locations. A composite sample can also be a representative sample taken at a
single sample point collected over an extended
time interval. Grab samples collected for further
preparation of a composite sample must be proportional. The time interval either between each
aliquot or between the volume of each aliquot
must be proportional to either the stream flow at
the time of sampling, or the total stream flow
since the collection of the previous aliquot.
Aliquots may be collected manually or automatically using specially designed equipment. SamPage 6-6

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ples that require analysis for VOAs should be


submitted to the laboratory as a grab sample
rather than a composited sample to minimize the
potential loss of the volatile contaminants.
6.6.1.

Operation of Sample Collection


Devices
Sampling personnel must be properly trained in
the operation of sample collection devices and
should review the manufacturers instructions
prior to sample collection. Sampling operations
must comply with all health and safety and
QA/QC requirements, and all sampling equipment must be properly cleaned and decontaminated between each collected sample.

sampling beaker. The adjustable clamp and


sampling beaker (stainless steel or Teflon) can be
obtained from most laboratory supply houses.
The sampler can also be constructed of a polyethylene cup with a pole that is joined in a single
fabrication.
Figure 6-1. Pond Sampler

6.6.1.1. Laboratory-Cleaned Sample Bottle


The most widely used method for collecting surface water samples is immersion of a laboratorycleaned sample bottle or certified pre-cleaned
bottle into the water to be sampled. Alternatively,
a laboratory-cleaned dipping bottle can be used to
fill sample bottles if immersion of the actual sample bottle is not feasible.
Sample Bottle Use Procedures
1. Ensure the bottles are intact, with proper fitting lids with linings that are compatible with
the contaminant under investigation.
2. Remove the lid, keeping it free from contamination during sampling. Immerse the bottle
into the surface water to the proper depth interval and allow the water to run slowly into
the bottle until it is full to zero headspace.
Replace the lid.
Note: Collect samples for VOC analysis first to prevent
loss of volatiles due to disturbance of the water. Section
6.6.2.1 discusses collection procedures for VOC samples.

6.6.1.2. Pond Sampler


The pond sampler (also called the dipper cup
sampler) is used to collect liquid samples from
disposal ponds, pits, lagoons, and similar reservoirs (see Figure 6-1). The sampler consists of an
adjustable clamp attached to the end of a two- or
three-piece telescoping aluminum tube, which
serves as the handle. Tubes can be readily purchased from most hardware or swimming pool
supply stores. The clamp is used to secure a
Chapter 6 Surface Water Sampling

Pond Sampler Use Procedures


1. Assemble the sampler in accordance with the
manufacturers instructions. Ensure the sampling beaker or sample bottle is clamped securely to the pole.
2. Slowly submerge the beaker with minimal
surface disturbance.
3. Retrieve the pond sampler from the surface
water with minimal disturbance.
4. Remove the cap from the sample bottle and
slightly tilt the mouth of the bottle below the
dipper edge.
5. Pour the sample slowly into the appropriate
sample container, allowing the sample stream
to flow gently down the inside wall of the
sample container with minimal entry turbulence.
6.6.1.3. Weighted Bottle Sampler
The weighted bottle sampler can be used to sample liquids from storage tanks, wells, sumps, or
other reservoirs that cannot be adequately sampled with another device (see Figure 6-2). The
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sampler consists of a bottle (usually glass) a


weight sinker, a bottle stopper, and a line used to
open the bottle and to lower and raise the sampler. This sampler uses a stainless steel or carbon
steel bottle basket that also serves as the weight
sinker.

Figure 6-3. Wheaton Dip Sampler

Figure 6-2. Weighted Bottle Sampler

Weighted Bottle Sampler Use Procedures


1. Assemble the sampler in accordance with the
manufacturers instructions.
2. Lower the sampling device to the predetermined depth.
3. When the sampler is at the required depth, pull
out the bottle stopper with a jerk of the sampler line and allow the bottle to fill completely.
(This is usually when air bubbles cease.)
4. Retrieve the sampler and transfer the sample
to the appropriate sample container.
6.6.1.4. Wheaton Dip Sampler
The Wheaton dip sampler is useful for collecting
liquid samples from shallow areas (see Figure 63). The sampler consists of a glass bottle mounted
on a metal pole of fixed length. Attached to the
bottles screw cap is a suction cup mounted on
another metal pole.

Chapter 6 Surface Water Sampling

Wheaton Dip Sampler Use Procedures


1. Assemble the sampler in accordance with the
manufacturers instructions.
2. Extend the device to the sample location, and
lower to the predetermined depth.
3. Turn the metal pole attached to the suction cup
to open the sample bottle.
4. When the bottle is full (usually when air bubbles cease), screw the cap back on to seal the
sampling container and retrieve the sample.
5. Transfer the sample to the appropriate sample
container.
6.6.1.5. Kemmerer Depth Sampler
The Kemmerer depth sampler is used to collect
liquid samples from lakes, storage tanks, tank
trailers, vacuum trucks, or anywhere collection
depth prevents the use of other sampling devices
(see Figure 6-4).
The Kemmerer depth sampler consists of an open
tube with two sealing end pieces or stoppers. The
end pieces can be withdrawn from the tube and
set in the open position until the sampler is at the
required sampling depth. Then, a weighted messenger is sent down the line or cable, releasing
the end pieces and trapping the sample within the
tube.

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Figure 6-4. Kemmerer Depth Sampler

Kemmerer Depth Sampler Use Procedures


1. Set the sampler so that the sealing end pieces
are pulled away from the sampling tube, allowing the water to pass through the tube.
2. Lower the sampling device to the predetermined depth. Avoid bottom disturbance.
3. Once the sampler reaches the required depth,
send down the messenger, closing the sampling device.
4. Retrieve the sampler, and discharge the first
10 20 milliliters from the bottom drain to
clear any potential contamination of the valve.
5. Pour the sample into the appropriate sample
container.
6.6.1.6. Bacon Bomb Sampler
The Bacon bomb sampler is a widely used, commercially available sampler designed for sampling liquids at a depth interval (see Figure 6-5).
The Bacon bomb sampler is constructed of brass
or stainless steel and is available in two sizes (1.5
inches or 3.5 inches in diameter with volumes
ranging from 4 or 32 fluid ounces, respectively).
The sampler is equipped with a spring loaded
trigger that allows liquid to enter the collection
chamber when opened. When the trigger is released, liquid is prevented from flowing into or
out of the collection chamber.

Chapter 6 Surface Water Sampling

Figure 6-5. Bacon Bomb Sampler

Bacon Bomb Sampler Use Procedures


1. Lower the sampler carefully to the desired
depth, allowing the line for the trigger to remain slack at all times. When the desired
depth is reached, pull the trigger line until taut.
This will allow the sampler to fill.
2. Release the trigger line, and retrieve the sampler.
3. Transfer the sample to the appropriate sample
container by pulling upon the trigger.
6.6.1.7. PACS Grab Sampler
The PACS grab sampler can be used to collect
liquid samples from lagoons, ponds, or containers
with restricted access (see Figure 6-6). For water
and liquid waste sampling, the narrow neck model is useful for maintaining the collected sample
inside of the device. The sampler consists of a
1,000-milliliter bottle screwed onto the end of a
6-foot fixed or telescoping handle.
PACS Grab Sampler Use Procedures
1. Assemble the sampler in accordance with the
manufacturers instructions.
2. Submerge the sampler into the liquid to be
sampled.
3. Once the sampler has reached the required
depth, open the sampler using the control
valve at the top of the handle.

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Figure 6-6. PACS Grab Sampler

4. After the sample is collected (usually when air


bubbles cease), close the sample bottle.
5. Retrieve the sampler.
6. Pour the sample into the appropriate sample
container.
6.6.1.8. Point Source Bailer
Point source sampling is performed to collect
samples from distinct levels or points of inflow.
To accomplish this task, a point source bailer can
be used that yields negligible disturbance and
mixing with water at different levels. This specially designed bailer has dual ball valves on both
the top and bottom of the sampling chamber to
isolate the sample at a discrete depth from mixing
with other depth intervals.
Point Source Bailer Sampler Use Procedures
1. Assemble the sampler in accordance with the
manufacturers instructions.
2. Lower the bailer slowly to the desired sample
depth on a support line. As the bailer is lowered, both ball valves are open, allowing the
water to flow through the sampler.
3. On reaching the sampling depth, the bailer is
raised using the support cable. The weight of
the water and upward movement of the bailer
keep both ball valves closed. The top ball
valve prevents the sample in the bailer from
mixing with water at higher levels.
Chapter 6 Surface Water Sampling

4. Once at the surface, the bailer is emptied by


opening the top vent and allowing the water to
drain slowly through the sample release device
into the sample container.
6.6.1.9. Automatic Samplers
An automated sampling system, consisting of a
pump, flow sensor, distribution system, and
sample containers can be used under appropriate
conditions for collecting point source samples.
An automated system is typically employed for
collecting a composite point source sample over
an extended time interval according to preprogrammed criteria. Automatic samplers can minimize labor requirements, reduce risk of human
error during sampling, and provide the opportunity for remote triggering of sampling according to
site conditions. Automatic sampling can be
limited by cost impact from equipment and installation, and potential for crosscontamination during sampler operation. The system is not appropriate for sample collection of sources that require analysis for VOCs and chlorine, as well as
microbiological agents, such as fecal coliform
and E. coli. Automated samplers are often customized for a specific project and site conditions.
Operating instructions should be developed and
implemented on a project-specific basis.
Use automatic samplers when several sites are to
be sampled at frequent intervals or when a continuous sample is required. Composite samplers
can be used to collect time composite or flow
proportional samples. In the flow proportional
mode, some samplers are activated by a compatible flow meter. Refer to your specific flow meter
operating manual for details on meter operation.
For older models, flow proportional samples can
be collected using a discrete sampler and a flow
recorder, and manually compositing the individual aliquots in flow proportional amounts.
6.6.1.9.1. Installing and Programming the
Automatic Composite Sampler
Use all new or pre-cleaned pump tubing each
time the sampler is brought to the field and set up.
Select tubing construction for the pump head and
sampling train according to the analytes of interest and the allowable construction materials.

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1. Cut the proper length of pre-cleaned Teflon


or Tygon tubing.
2. Collect equipment blanks at a frequency of 5%
of the samples by passing analyte-free water
through the equipment that is exposed to the
sample.
3. Put the collection sieve and tubing in the
appropriate sample location in the wastewater
stream, using conduit if necessary to hold it in
place. Ensure the supporting conduit does not
contaminate the incoming sample water.
4. Program the sampler per manufacturers directions and as required in the permit or work
plan conditions.
5. For a time composite sample, program the
sampler to collect a minimum of 100 mL for
each sample interval. Adjust the volume collected according to the duration of the sampling event, the sampling interval, and the size
of the container.
6. For a flow proportional sample, program the
sampler to collect a minimum of 100 mL for
each sample interval, with the interval predetermined based on the flow of the waste
stream.
7. Automatic Sampler Security: A lock or seal
may be placed on the sampler to prevent or
detect tampering. However, this procedure
does not prevent tampering with the sampler
tubing.
6.6.1.9.2. Sample Acquisition
1. At the end of each sampling period, stir the
contents of the compositing jug (sample) and
siphon contents (poured if no visible solids)
into the appropriate sample containers. If the
sampler was set up to collect discrete samples,
ensure that the contents of each container are
adequately mixed while pouring the sample
into the sample container.
2. Immediately preserve the sample; if required,
cap and label the sample container.
6.6.1.9.3. Long-Term Deployment of
Automatic Composite Samplers
In certain sampling situations, automatic composite samplers are permanently installed at the
sample stations and remain in the field for months
Chapter 6 Surface Water Sampling

or even years. Under these conditions, there are


specific sampling issues that need to be addressed.
6.6.1.9.4. Sample Preservation
1. If the only analyte of interest is Total Phosphorus, and the project is unrelated to an NPDES
permit, the sample must be chemically preserved with sulfuric acid (H2SO4) but does not
need to be cooled to 6Cwith wet ice. Other
analytes will need chemical preservation and
cooling.
2. The acid must be in the container prior to
drawing the first composite sample into the
container. When using large (i.e., 3-gallon)
composite sample containers, and there is potential for the sample size to vary greatly due
to variable flow rates at the site, the volume of
acid for preservation should be small (e.g., 1
2 mLs of 50% H2SO4). Do not over acidify
the sample. Upon sample pick-up, if needed,
add additional acid to achieve the proper pH
adjustment (i.e., pH 2) for preservation.
3. Cool samples with ice or refrigeration.
6.6.1.9.5. Cleaning Requirements
1. Clean composite sampler containers after
collection of each composite sample using
cleaning solutions and procedures.
2. Composite sample containers may be cleaned
either in the field or in a fixed-base operation.
Demonstrate cleaning effectiveness by collecting equipment blanks on the composite sample
containers according to the frequency specified by the manufacturer. Typically, collect
sampler container equipment blanks by adding
a minimum of 1 L of analyte-free water to the
cleaned sample container, mix the water thoroughly within the container, and then pour off
an aliquot for analysis.
3. Replace tubing at a minimum of every six
months. Inspect the tubing each time the
composite sample container is picked up. If
there is evidence of loss of elasticity or discoloration or other conditions (such as algal
growth) that would impact the quality of the
sample, then replace the tubing prior to the end
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ment blank each time new tubing is installed in


the auto sampler. Collect this equipment blank
by passing analyte free water through the entire length of the new tubing being deployed at
each station. If the tubing is being replaced for
multiple autosamplers at the same time, one
equipment blank may be collected on the entire length of replacement tubing. Collect this
equipment blank by passing analyte-free water
through the entire length of new tubing.
6.6.1.10. Summary of Surface Water Sampling
Devices
A summary of collection devices that are designed for collecting surface samples, including
their advantages and disadvantages for use, are
presented in Table 6-1.
6.6.2. Sample Collection Procedures
For detailed sampling procedures and preservation of samples, refer to Appendix B of this
handbook. It is important to remember that COC
procedures should be followed for all surface
water sampling events and that all samples are to
be preserved with ice to 4 2C during both
sample collection and shipment to the laboratory.
Details regarding the use of COC procedures are
provided in Chapter 3.
6.6.2.1. Sampling for VOCs
Use the following procedures for collecting samples for VOCs:
1. Remove the cap from a 40-millileter septum
(Teflon-lined silicon rubber) vial. Avoid
contact with the inner surface.
2. Add the established amount of HCl necessary
for sample preservation (if pre-preserved vials
have not been supplied by the laboratory, prepreserved vials cannot be used if the actual
VOC collection container is dipped into the
water being sampled).
3. Fill the vial with sample water, taking care to
minimize aeration, and screw the cap on tightly
to achieve zero headspace.
4. If effervescence occurs due to high carbonate
salts in the samples, do not add acid preservative, and contact the Project Manager for ap-

Chapter 6 Surface Water Sampling

propriate actions such as reduced sample holding times.


5. Inspect the vial for air bubbles. If air bubbles
are present, discard the sample and restart with
step 1.
6. Label the vial, and place it in a resealable bag.
Place the sample vials in a cooler with bagged
ice sufficient to cool to 4 2C.
7. Record all appropriate data in the FLB/FN.
6.6.2.2. Samples for SVOCs
Use the following procedures for collecting samples for SVOCs:
1. Remove the Teflon-lined cap from a 1-liter
amber glass bottle. Avoid contact with the inner surface of the cap.
2. Fill to the neck of the bottle with surface water.
Add chemical preservatives, if required by the
permit or method. Record the amount, type of
preservative, and other preservation data per the
SAP. Pre-preserved bottles also may be used
for sampling surface water for extractable organics analysis, unless the sample is collected
directly into the container.
3. Replace the cap tightly, attach the sample label,
and place the sample bottle in a cooler with
bagged ice sufficient to cool to6C.
4. Fill additional bottles by repeating steps 1 3.
5. Record all appropriate data in the FLB/FN.
6.6.2.3. Sampling for Additional Parameters
1. Remove the cap from the sample bottle. Avoid
contact with the inner surface of the cap.
2. Fill about 90 percent of the bottle with surface
water, and preserve to a pH of < 2 with nitric
acid. Pre-preserved sample bottles also may be
used for metals analysis.
3. Record the amount, type of preservative, and
other preservation data per the SAP. Replace
the cap tightly, attach label, and place the
sample bottle in a cooler with bagged ice sufficient to cool to6C, if required by the permit or method.
4. Fill additional bottles by repeating steps 1 3.
5. Record all appropriate data in the FLB/FN.

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6.6.2.4. Sampling for Additional Parameters


1. Remove the cap from the sample bottle.
Avoid contact with the inner surface of the
cap.
2. Fill the bottles per the SAP or method requirements.
3. Add the appropriate preservative to the samples, if required.
4. Replace the cap tightly.
5. Attach label.
6. Place sample bottles in a cooler with enough
bagged ice to cool them to6C, if necessary.
7. Record all appropriate data in the FLB/FN.
6.7. Sampling Equipment List
Section 3.8 provides a generic sampling equipment list applicable to most sampling events. The
following list provides additional specific equipment that may be applicable to surface water
sampling.

Preservation chemicals and reagents


pH meter, DO meter, conductivity meter, and
thermometer
Sample collection devices
- Pond sampler
- Weighted bottle sampler
- Wheaton dip sampler
- Kemmerer depth sampler
- Bacon bomb sampler
- PACS grab sampler
- Point source bailer
- Automatic sampler system
Stainless steel tape and measuring rod
Field blanks
Trip blanks when measuring VOCs
Cleaning materials and reagents
Decontamination materials and detergent
Dedicated, pre-cleaned dipping devices or
bottles, if necessary.

Chapter 6 Surface Water Sampling

Table 6-1. Sampling Devices for Collecting


Surface water
Collection
Device

Advantages

Laboratory Easy to use.


Low contamination
-Cleaned
risk.
Sample
No decontamination
Bottle
required.

Disadvantages
Difficult to label wet
bottle.
Pre-preserved bottles
cannot be used.
Exterior of bottle may
contact the sample.

Pond
Sampler

Easy and inexpensive Difficult to obtain a


to fabricate.
representative sample in
Samples to depths of
stratified liquids.
3.5 meters.
Difficult to
decontaminate when
viscous liquids are
encountered.

Weighted
Bottle
Sampler

Can be fabricated or
purchased.
Remains unopened
until it reaches
sample depth.

Wheaton
Dip
Sampler

Allows discrete
Sampling depth is limited
samples to be taken at by the length of the
depth.
poles.
Exterior of bottle may
contact the sample.

Kemmerer
Depth
Sampler

Ability to sample at
Sampling tube is exposed
various and great
to water while traveling
depths.
down to sampling depth.
Allows discrete
samples to be taken at
depth.

Bacon
Bomb
Sampler

Allows discrete
Difficult to
samples to be taken at decontaminate.
If brass construction,
depth.
may not be appropriate in
metals analysis or
toxicity testing.
Difficult to transfer
sample to container.
The sample can become
aerated.

PACS
Grab
Sampler

Allows discrete
Depth of the sampling is
samples to be taken at limited by the length of
depth.
the pole.
Difficult to
decontaminate.

Point
Source
Bailer

Allows discrete
May be difficult to
samples to be taken at operate.
Difficult to
depth.
decontaminate.

Automated
Sampler

Allows discrete
Not appropriate for
samples to be taken at collecting samples
depth.
requiring VOC and
microbiological analysis.

May be incompatible
with some liquids.
Laboratory-supplied
bottle may not fit into the
sampler.
Mixing of the sample
may occur.

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Chapter 6 Surface Water Sampling

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Chapter 7. Storm Water Sampling


7.1. Purpose
Military bases and other federal facilities are
regulated under the NPDES storm water program.
The industrial permit program, the Municipal
Separate Storm Sewer Systems (MS4) permit
program, and the Construction Activities Permit
Program may apply to military bases and other
federal facilities. See Section 7.2 for an overview
of Phase I and II storm water regulations. The
following classes of discharges are regulated
under NPDES storm water permit coverage:

Operators of MS4s located in urbanized areas


(UAs) or where designated
Industrial facilities in any of the 11 categories
that discharge to an MS4 or to waters of the
United States. All categories of industrial
activities (except construction) may certify to a
condition of no exposure if their industrial
materials and operations are not exposed to
storm water, eliminating the need to obtain
storm water permit coverage.
Operators of construction activities that disturb
one or more acres of land and construction
sites less than one acre are regulated if part of
a larger plan of development.
Storm water sampling at MS4s, industrial facilities and construction sites, including those at
DoD installations, may be required to verify
permit compliance. The need for storm water
sampling will be determined based on the type of
permit the facility obtains. For example, if a DoD
industrial facility is located within a state that
uses the Multi-Sector General Permit (MSGP),
then analytical monitoring of outfalls associated
with specific industrial sectors is required quarterly during permit years two and four. Other
states may issue a general storm water permit,
which requires sampling only for specific types of
industrial activities. Each permit provided to the
facility will outline the specific sampling and
analysis requirements. This is the first step to
determine:

Sampling requirements
The outfalls to be monitored
Chapter 7 Storm Water Sampling

The types of samples that need to be collected


(e.g., grab vs. composite, first flush)
The types of pollutants to be analyzed.
This chapter provides an overview of the:
Federal storm water regulations including
permitting requirements
Activities at DoD facilities that may impact
storm water
Compliance monitoring strategies including
sampling and analysis, QA, and health and
safety requirements for storm water
monitoring
Commercially available equipment used for
storm water monitoring.
7.2. Storm Water Program Overview
This section provides an overview of the federal
storm water program including the differences
between Phases I and II of the regulation, and
permitting options for both industrial facilities
and construction sites. A detailed description of
the storm water regulations and permitting steps
for DoD facilities can be found in the U.S. Army
Environmental Centers Storm Water Guidance
Manual, dated July 27, 2005.
7.2.1. Regulatory Summary
The CWA was amended in 1972 to prohibit discharges of any pollutant to waters of the United
States from point sources 1 unless that discharge
was authorized by a NPDES permit. Originally,
EPA efforts to track point sources and improve
water quality under the NPDES program focused
on reducing pollutants in industrial wastewater and
municipal sewage. Studies in the late 1980s,
however, indicated that while wastewater regula1

A point source is defined under 40 CFR 122.2 as any


discernible, confined, and discrete conveyance, including
but not limited to, any pipe, ditch, channel, tunnel, conduit,
well, discrete fissure, container, rolling stock, concentrated
animal feeding operation, landfill leachate collecting system,
or vessel or other floating craft from which pollutants are or
may be discharged. Since the definition of a point source is
broad and can vary among individual states, installation staff
should contact the appropriate NPDES permitting authority
to verify a point source discharge.
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tions had dramatically decreased the amount of


pollutants in the nations waters, these waters were
still polluted. The major source of pollutants
entering the waterways was determined to be from
storm water runoff rather than from industrial or
municipal discharges. Utilizing the CWA
amendments of 1987, EPA promulgated NPDES
Phase I storm water regulations in 1990 and Phase
II regulations in 1999 to address storm water
runoff from point sources (excluding agricultural
runoff). These point sources include storm water
runoff from MS4s, storm water discharges from

certain industrial activities, and storm water


runoff from construction activities. Figure 7-1
provides an overview of the NPDES storm water
regulations. Specific requirements for the Phase I
and Phase II rules are described below.
Additionally, Section 303(d) of the CWA, requires that states develop lists of impaired waters
and establish Total Maximum Daily Loads
(TMDL) for those waters. A TMDL is a calculation of the maximum amount of a pollutant that a
water body can receive and still safely meet water
quality standards.

Figure 7-1. Overview of NPDES Storm Water Regulations

Chapter 7 Storm Water Sampling

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7.2.1.1. Phase I Regulations


The NPDES Phase I regulations require the
following types of activities and systems to
obtain storm water discharge permits:

Industrial activities in 11 categories


Construction activities disturbing five or more
acres of land
Medium MS4s (serving populations of
100,000 250,000)
Large MS4s (serving populations > 250,000)
No exposure exemption for light industry.

7.2.1.2. Phase II Regulations


The Phase II program expanded Phase I by
requiring storm water discharge permits from the
following activities and systems:

Small MS4s (populations < 100,000) in UAs


Municipal industrial facilities similar to those
under Phase I
Small construction sites disturbing one to five
acres
Construction activities disturbing less than
one acre if the site is part of a larger common
plan of development or sale
Two new classes of discharges: 1) particulate
matter from roof stacks and vents not
otherwise regulated; and 2) visible track out
or windblown raw materials.
This storm water sampling chapter will focus on
both DoD industrial facilities and large and small
construction activities at DoD installations.
Information on storm water sampling at MS4s is
beyond the scope of this document.
7.2.2. Permitting Requirements
A number of DoD facilities conduct industrial
operations that require storm water permitting.
Some of these operations include munitions
manufacturing (e.g., chemical plants), metal
fabrication and plating, equipment maintenance,
power generation, fuel transfer and storage, and
waste management areas. Regulated industrial
activities at DoD facilities may be covered by an
individual storm water permit or a General
Storm Water Permit (GP) from either EPA or the
Chapter 7 Storm Water Sampling

state environmental agency. An individual


permit can be more intensive, with more sitespecific requirements, while the GP application
process and permit requirements are usually
more streamlined and less stringent. Specific
permit requirements vary depending on permit
type and EPA or state requirements. States with
NPDES permitting authority may impose more
stringent requirements or expand the scope of
their programs to meet state priorities or watershed requirements.
Construction activities at DoD facilities must
also comply with storm water permitting requirements. Two types of storm water permits
are available for construction activities. A GP,
which is typically used for construction activities, and less commonly, an individual permit.
EPA and states encourage developers, construction contractors and federal facilities to apply for
construction GPs when necessary, although there
may be certain situations where the permitting
authority would require an individual permit.
For example, if the operator of a construction
activity is proposing to discharge an unallowable
non-storm water discharge into an impaired
water body, then the permitting authority may
require coverage under an individual permit.
EPA defined a regulated construction activity in
the Phase I storm water rules to include:
all clearing, grading, and excavation
activities, except operations that result in
the disturbance of less than 5 acres of total
land area. Construction activity also includes the disturbance of less than 5 acres
of total land area that is part of a larger
common plan of development or sale if the
larger common plan will ultimately disturb
5 acres or more...
This definition was expanded by the Phase II
requirements to include small construction activities that disturb one to five acres of land, or less
than one acre if the construction activities are
part of a common development or sale (40 CFR
122.26(b)(15)).

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Various ground-disturbing projects at DoD


facilities are considered to be regulated construction activities and would require a storm water
construction permit and sampling if they disturb
one or more acres of land, and result in a point
source discharge into waters of the United
States. Typical installation construction activities may include but are not limited to:

Clearing of an area to construct a new


munitions plan
Grading activities associated with demolition
or remediation
New road construction or full-depth reconstruction of existing roads
Construction of housing units, offices,
training facilities, or commissaries
Combat Engineer Company training
activities.

Coverage under the federal Construction General


Permit (CGP) authorizes the permittee to discharge the following during construction, provided that all terms of the permit are being met:

Storm water discharge associated with


construction activities from either large or
small construction sites including storm water
discharge that disturbs less than one acre that
is part of a larger common plan of
development or sale that, when combined,
disturbs one acre or more
Storm water discharge from sites disturbing
less than one acre, but designated by EPA as
needing coverage under the CGP
Storm water discharge from construction site
support activities directly related to the
construction site with CGP coverage (e.g.,
concrete or asphalt batch plants, equipment
staging yards, material storage areas, trackout roadways, etc.)
Any discharge authorized by a different
NPDES permit commingled with discharge
authorized by the CGP.
Additionally, the federal CGP authorizes the
following non-storm water discharge, if the nonstorm water component of the discharge is in
Chapter 7 Storm Water Sampling

compliance with Subpart 3.5 (Non-Storm Water


Discharge Management) of the CGP:

Discharge from fire-fighting and fire hydrant


flushings
Water used for vehicle and external building
washing where detergents are not used
Water used to control dust in accordance with
Subpart 3.4.G of the CGP
Potable water, including uncontaminated
water line flushing
Pavement wash water where spills or leaks of
toxic or hazardous materials have not
occurred (unless all spilled material has been
removed) and where detergents are not used
Uncontaminated air conditioning or
compressor condensate
Uncontaminated groundwater or spring water
Foundation or footing drains where flows are
not contaminated with process materials
Uncontaminated excavation dewatering and
landscape irrigation.

All other discharges associated with the construction activity are prohibited by the CGP and
will require coverage under an individual storm
water permit or another type of NPDES permit.
7.3. Storm Water Compliance
The intent of the Phase I and Phase II regulations
are to prevent storm water from becoming contaminated by industrial or construction activities,
rather than requiring quantitative monitoring of
storm water outfalls. To implement the intent of
the regulation, the control authority (EPA or the
state) requires a systematic approach be taken to
identify the facilitys potential storm water
impacts, and to mitigate these impacts through a
series of best management practices (BMPs).
BMPs can be either non-structural or structural.
Non-structural BMPs include procedural
changes such as not allowing off-loading of fuel
during rain events, covering of storm-drains
during material transfer, or not storing materials
outside. Structural BMPs are physical changes
to the facility or implementation of technologies
to prevent pollutants from leaving an industrial
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facility or construction site. Structural BMPs


may include items such as check-dams for controlling runoff and trapping sediment, storm
water retention ponds for capture of sediment,
and storm drain valves to prevent releases from
leaving a facility.
The first step in the systematic process to prevent
contaminated storm water from leaving the
industrial facility or construction site requires
development of a storm water pollution prevention plan (SWPPP). The SWPPP describes
issues such as potential locations for storm water
contamination, possible pollutants, drainage
patterns, outfalls, and BMPs that could be established to prevent polluted runoff. The storm
water permit, along with information gathered
during preparation of the SWPPP, provide
DoDs environmental staff with the information
needed to develop a compliance monitoring
program for the site.
The remainder of this section discusses SWPPP
development for both industrial facilities and
construction sites. It provides insight into the
types of pollutants expected at DoD industrial
facilities and construction sites, and the current
technologies and techniques being used to verify
compliance through either visual monitoring or
collection and analysis of storm water samples.
7.3.1. Development of a SWPPP
Preparation of a pollution prevention plan is the
first step toward compliance with the storm
water regulations. The SWPPP identifies the
sources and types of storm water pollution associated with all industrial and construction activities covered under the GP/Individual Permit. It
describes the BMPs that the installation will
implement to reduce or eliminate pollutant
sources and describes the monitoring requirements to verify compliance. The bullets below
describe information that is provided in the
primary sections of an SWPPP. See EPAs
Storm Water Management for Industrial Activities: Developing Pollution Prevention Plans and
Best Management Practices, for more guidance
on preparing an SWPPP for industrial discharges.
Chapter 7 Storm Water Sampling

Pollution Prevention Team. The first step in


developing and implementing an SWPPP is to
identify a qualified individual or team of
individuals who will be responsible for
developing the plan and assisting with
implementation. This team should represent
all relevant departments in the industrial areas
covered by the permit. The plan must
describe the responsibilities of each team
member as they relate to specific components
of the plan.
Description of the Facility and Potential
Pollution Sources. The SWPPP must
identify the activities, materials, and physical
features of the regulated activity at the
installation that may contribute significant
amounts of pollutants to storm water runoff,
or may result in pollutant discharges through
a separate storm sewer system or storm water
drainage system during dry weather. If there
is a significant amount of pollution running
onto the facility from an adjacent property,
addressing or diverting this run-on should be
addressed in the SWPPP. If it cannot be
addressed, the permitting authority should be
notified.
Description or Map of Site and Receiving
Waters/Wetlands. The map must include
the location of all outfalls covered by the
NPDES permit. It must also denote the storm
water drainage patterns, locations where
significant materials are exposed to rainfall
and runoff, locations of major spills and leaks
that have occurred in the drainage areas of the
permitted outfalls within 3 years prior to
receiving the Notice of Intent (NOI) to
discharge storm water; and other installationspecific information.
Summary of Potential Pollutant Sources.
Provide a narrative description of activities,
materials, and physical features of the
installation that are potential pollutant sources
affecting storm water quality. Describe areas
of the installation that are subject to reporting
under Section 313 of EPCRA.

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Significant Spills and Leaks. Provide a list


and description of cause, type, volume,
location, and response actions taken for each
significant spill or leak of toxic or hazardous
pollutants that occurred within 3 years prior to
the date of the submission of the NOI.
Allowable and Prohibited Non-Storm
Water Discharges. Include a certification
signed by an authorized individual to affirm
that discharges from the installation have been
tested or evaluated for the presence of nonstorm water discharges. The certification
ensures that the installation is only
discharging non-storm waters allowable under
the GP.
Selection and Implementation of Storm
Water Controls. Evaluate, select, and
describe the pollution prevention measures,
BMPs, and other controls that will be
implemented at the installation to control
storm water pollutants. The appropriateness
of each selected control and how each control
will address one or more of the potential
pollution sources identified must be
explained. This includes discussing how the
individual controls relate to one another as a
whole, and producing an integrated approach
for preventing and controlling storm water
pollution.
Storm Water Monitoring Requirements.
Monitoring requirements must be detailed in
the SWPPP. Monitoring requirements will be
detailed in the storm water permit provided by
the regulatory authority and will range from
visual monitoring of storm water to collection
and analysis of storm water samples. The
storm water monitoring section must also
include a schedule that details the frequency
that storm water monitoring must be
performed.
Internal Reporting of Storm Water
Information. A reporting system must be
established to ensure timely reporting of
storm water management-related information
to appropriate installation personnel. A

Chapter 7 Storm Water Sampling

description of the reporting system must be


included in the SWPPP.
Copy of Permit. A copy of the permit
language and the confirmation letter received
from the NOI processing center must be
included with the SWPPP.
Certification. The SWPPP must be signed
and certified by the ranking officer of the
installation, such as the commander or his or
her duly authorized representative (an
individual or a position). The representative
is only duly authorized if the ranking officer
documents it in writing and provides this
letter to the permitting authority.
The SWPPP, along with the permit language,
will help the environmental staff at a DoD facility evaluate the proper monitoring requirements
for their storm water. Information collected
while developing the SWPPP will help the onsite environmental staff choose the storm water
monitoring locations and identify the pollutants
that can be reasonably expected in storm water
runoff. Information in the storm water permit
provided by the control authority will help the
environmental staff determine the types of monitoring that must be conducted to verify compliance (e.g., visual observations, sampling) and
the frequency of monitoring.
7.3.2.

Compliance Monitoring at Industrial


Sites
Storm water regulated by the Phase I and Phase
II rules are typically generated by either industrial or construction activities at DoD facilities.
Industrial activities are identified by specific
Standard Industrial Classification (SIC) codes.
Other operations with no designated SIC code,
such as landfills or hazardous waste treatment
storage and disposal facilities, require permitting
if other additional industrial activities occur at
the facility are permitted. Although there is no
specific SIC code that applies to all DoD facilities, the Phase I regulations state that EPA intends to address DoD facilities engaged in industrial activities as federal facilities that meet the
description of the facilities listed in the regulation (53 FR 49416, 49432; 07 December 1988).
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Table 7-1 lists some of the industrial-type activities common at DoD facilities that may require

storm water permitting and possibly compliance


sampling.

Phase I Industrial
Classification

Classification Under 2000 MSGP

Additional
SWPPP Reqs.b

Industrial Activity at DoD


Installations

Chemical
Samplinga

Table 7-1. Potential Industrial Activities at DoD Installations with Storm Water Considerations

Motor Pools

(viii) Transportation facilities.


Only if related to another
regulated industrial activity at
the facility.

Although motor pools alone are not considered


Sector P with regard to monitoring requirements,
they are still considered an industrial activity and
must be covered by the SWPPP if any other
industrial activity requires the facility to obtain a
Phase I permit.

Yes No

Airfields

(viii) Transportation facilities. Sector S. Installation needs permit coverage if


Only if maintenance, cleaning, aircraft maintenance, equipment cleaning, or
or deicing activities occur.
deicing occurs regardless of amount of fluid
used. Deicing areas include runways, taxiways,
ramps, gates, and areas where planes are deiced.
Sector monitoring requirements do not apply if
installation uses < 100,000 gallons of glycolbased fluid per year, or < 100 lbs. of urea/yr.

Yes Yes

Wastewater Treatment
Plants

(ix) Treatment works. Design


flow > 1.0 million gallons per
day (MGD) or are required to
have an approved pretreatment
program.

Sector T, Treatment Works. Applies only if unit No Yes


has design flow > 1.0 MGD or is required to have
an approved pretreatment program.

Hazardous Waste TSDFs

(iv) Hazardous waste. Only


for facilities requiring a RCRA
permit.

Sector K. Only if installation has a RCRA


permit. This includes hazardous waste landfills.

Open Burn/Open Detonation Sites

(iv) Hazardous waste. Only if Sector K. Only if the installation has a RCRA
RCRA permitted facility.
permit.

Department of Logistics
Terminals/ Loading Facilities

(xi) Light industry.

Tech Shops with Electroplating Operations

(i) Facilities subject to effluent Sector AA. Produces plated ware or fabricated
metal products, except for electrical-related,
limitation guidelines.
machinery, and transportation equipment.

Tech Shops with Metal


Fabrication Operations

(xi) Light industry.

Sector AA. See above.

Yes Yes

Ammunition/Ordnance
Production Operations

(xi) Light industry.

Sector AA. See above.

Yes Yes

Missile & Missile Parts


Production

(xi) Light industry.

Sector AB. Produces industrial and commercial


machinery or transportation equipment.

No Yes

Aircraft Parts Fabrication

(xi) Light industry. If not


associated with an airfield, or
(viii) Transportation. If
associated with an airfield.

Sector AB. If not associated with an airfield, or


Sector S if associated with an airfield.

No Yes

Tech Shops with Electrical

(xi) Light industry.

Sector AC.

No

Chapter 7 Storm Water Sampling

None.

Yes No

Yes No
No

No

Yes Yes

No

Page 7-7

Phase I Industrial
Classification

Classification Under 2000 MSGP

Additional
SWPPP Reqs.b

Industrial Activity at DoD


Installations

Chemical
Samplinga

DoD Environmental Field Sampling Handbook


Revision 1

Component/ Equip. Production


Sector O. Facilities that generate steam electric
power using coal, oil, natural gas, nuclear power
or dual-fuel co-generation facilities.

Yes Yes

Operations that Print &


(xi) Light industry.
Publish DoD or Installation
Documents, Periodicals,
Newspapers

Sector X.

No Yes

Misc. Service & Repair


None.
Shops, Including Electrical
Shops, Furniture, Refrigeration, & Privately Owned
a
Chemical sampling is required only if the installation
meets the definition of the SIC code.
b
The MSGP specifies additional information that must
be included in the SWPPP for these sectors.

None.

N/A N/A

Steam Electric Power


Generating Stations

(vii) Steam electric power


generating facilities.

7.4. Visual Monitoring of Storm Water from


Industrial Facilities
The majority of storm water monitoring at DoD
industrial facilities will be audited for structural
and non-structural BMPs, visual monitoring of
outfalls for dry-weather flows, and visual water
quality monitoring of outfalls during storm events.
Visual monitoring requirements will be outlined in
either the GP or the individual permit and should
be included in the SWPPP, along with the locations of BMPs and storm water outfalls, drainage
patterns, and potential industrial-type pollutants
that could be expected based on material storage
and use at the facility.
Visual monitoring of storm water outfalls during
dry weather situations are conducted to determine
if there are illicit connections to storm sewers that
may result in the non-permitted discharge of industrial wastewater, sanitary water, non-contact cooling waters, condensates, blow down, foundation
drains (i.e., groundwater) or other types of water
used at the facility. If dry-weather visual monitoring discovers flow at storm water outfalls, then
visual characterization of the discharge should be
recorded to help identify the source.

Chapter 7 Storm Water Sampling

Some characteristics that are helpful in identifying


the source of the dry-weather flow include:

Color and odor


Turbidity
Temperature
Oil sheen
Foam
Floating particulates (e.g., paint, plastics).
If the source of the non-permitted discharge is not
identified by visual observations, then collection
and analysis of grab or composite samples of the
dry-weather flow may be required to identify the
source. Once the source of the dry-weather flow
has been identified, either the illicit connection to
the storm sewer must be removed or the facility
must obtain a NPDES permit for discharge from
the source to surface water through the storm
water outfall. Figure 7-2 is a sample checklist,
reproduced from EPAs NPDES Storm Water
Sampling Guidance that can be used for dry
weather visual observations.
7.5. Collection of Storm Water Samples
Data that characterize storm water discharge are
valuable to permitting authorities and the permitPage 7-8

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ted facility for several reasons. First, storm water


sampling provides a means for evaluating the
environmental risk of the storm water discharge by
identifying the types and amounts of pollutants
present. Evaluating these data helps determine the
relative potential for the storm water discharge to
contribute to water quality impacts or water quality
standard violations. In addition, storm water
sampling data can be used to identify potential
sources of pollutants. These sources can then be
either eliminated or controlled more specifically
by the permit.

fissure, container, rolling stock, concentrated


animal feeding operation, landfill leachate collection system, vessel, or other floating craft from
which pollutants are or may be discharged (as per
40 CFR 122.2). Included in the definition of storm
water point source is storm water from an industrial facility that enters, and is discharged through
a municipal separate storm sewer. In short, most
storm water discharges can be defined as point
source discharges, since they ultimately flow into
some form of conveyance such as a channel or
swale.

Industrial group or individual permitees that are


required to collect samples must follow specific
storm event criteria to ensure the analytical results
are representative. EPAs criteria for sampling a
storm event are listed below:

Industrial facilities with a general permit or individual permit that requires compliance sampling
are usually required to collect and analyze a grab
sample taken within the first 30 minutes of a storm
event and flow-weighted composite samples from
each of the industrial storm water point source
outfalls identified in the Storm Water Pollution
Prevention Plan (SWPPP). If possible, all outfalls
should be sampled during the same representative
storm event. The descriptions of each storm event
and the outfalls sampled must be recorded.

The storm must result in > 0.1 inch


accumulation
The storm must be preceded by 72 hours of dry
weather
Where feasible, the depth of rain and duration
of the event should not vary by more than 50
percent from the average depth and duration.
These criteria were established to: 1) ensure that
adequate flow would be discharged; 2) allow for
build-up of pollutants during dry weather intervals;
and 3) ensure that the storm would be representative, i.e., typical for the area in terms of intensity,
depth and duration. Data collected from the storm
event may include the following:

Total discharge volume


Rainfall duration
Maximum flow rate
Rainfall amount
Method of flow measurement (or estimate)
Time from the last date that 0.1 inches of rain
fell
Date of the storm event.
Storm water samples should be taken at a storm
water point source. A point source is defined as
any discernible, confined, and discrete conveyance, including (but not limited to) any pipe,
ditch, channel, tunnel, conduit, well, discrete
Chapter 7 Storm Water Sampling

7.5.1. Sampling Locations


The ideal sampling location would be the lowest
point in the drainage area where a conveyance
discharges storm water to waters of the United
States or to a municipal storm sewer system. This
sample point should also be easily accessible on
foot in a location that will not cause hazardous
sampling conditions. Ideally, the sampling site
should be on the applicants property or within the
municipalitys easement. If not, the field personnel should obtain permission from the owner of the
property where the discharge outfall is located.
Typical sampling locations may include the discharge at the end of a pipe, a ditch, or a channel,
however, logistical problems with sample locations may arise (e.g., nonpoint discharges, inaccessibility of discharge point, etc.). Logistical problems with sample locations and suggested solutions are described in Figure 7-3 . In many cases,
it may be necessary to locate the sampling point
further upstream of the discharge point, such as in
a manhole or inlet. If the storm water at a selected
location is not representative of a facilitys total
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runoff, the facility may have to sample at several


locations to best characterize the total runoff from
the site. In situations where discharge points are
difficult to sample, the permitted facility should
take the best sample possible and explain the
conditions in the documentation maintained with
the SWPPP.
7.5.2. Staffing Considerations
Staffing needs for sampling must be determined by
the permitted facility. Factors in making the determination include the number of sample locations, the size of the area to be sampled, how far
apart the locations are, the type of sampling required, the technique to be used, the number of
samples to be taken (depending on how many
parameters must be analyzed), and safety considerations. Sampling training is important to the
success of storm water discharge characterization.
Sampling conducted by untrained personnel may
result in data that is unrepresentative of the individual facilities storm water discharge. This data
may be rejected by a permitting authority, which
would then require another sampling effort.

Chapter 7 Storm Water Sampling

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Figure 7-2. Checklist for Conducting Dry Weather Evaluations


1.
3.
4.
5.

Date of Inspection:
End Date of last rain event:
Inspector name:
Type of outfall
Concrete Pipe
Grassed
Rock
Other

2. Facility name and address:

6.

Is there viable flow from the pipe?


Yes No
If yes, check all that apply. If no, go to
number 7.
Colored water (describe)
Oily sheen
Odor* (describe)
Sludge present
Murky
Clear water
Floating objects (describe)
Stains on conveyance
Absence of plant life surrounding
Notable difference in plant life surconveyance
rounding conveyance
Scum
Suds Other:
*e.g., rotten eggs, earthy, chemical, chlorine, soap, putrescence, gasoline, musty, etc.
Estimate the flow either visually or by describing the width, height, and shape of the
conveyance and the approximate percentage of the conveyance where flow is present or
the approximate depth of the flow. Describe your estimate.
7. Is there standing water present?
Yes No
If yes, check all that apply. If no, go to
number 8.
Colored water (describe)
Oily sheen
Odor* (describe)
Sludge present
Murky
Clear water
Floating objects (describe)
Stains on conveyance
Absence of plant life surrounding
Notable difference in plant life surconveyance
rounding conveyance
Suds
Scum Other:
*e.g., rotten eggs, earthy, chemical, chlorine, soap, putrescence, gasoline, musty, etc.
8. From the inspection locations, can you see any unusual piping or ditches that drain to
the storm water conveyance?
Yes No
9. Is there any overload flow visible from the discharge location? Yes No
10. Are there dead animals present?
Yes No
Signature:

Chapter 7 Storm Water Sampling

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Figure 7-3. Solutions to Sampling Location


Problems
Problem:
Solution:

Problem:
Solution:

Problem:

Solution:

Problem:

Solution:

Problem:
Solution:

Sampling where storm water commingles with


process or non-process water.
Attempt to sample the storm water discharge
before it mixes with the non-storm water
discharge. If this is not possible, sample the
discharge during dry and wet weather and
present both sets of data to the permitting
authority. This will provide an indication of the
contribution of pollutants from each source.
Numerous small point discharges.
Impound channel or join flow by building a
weir or digging a ditch to collect discharge at a
low point for sampling purposes. This artificial
collection point should be lined with plastic to
prevent infiltration and/or high levels of
sediment. Or, sample at several locations to
represent total site runoff.
Inaccessible discharge point, such as underwater
discharges or unreachable discharges (e.g., out of
a cliff).
Go up the pipe to sample, i.e., to the nearest
manhole or inspection point. If these are not
available, tap into the pipe or sample at several
locations to best represent total site runoff.
Managing multiple sampling sites to collect
grab samples during the first 30 minutes (industrial facilities only).
Have a sampling crew ready for mobilization
when forecasts indicate that a representative
storm will occur, or sample several different
representative events. For most parameters,
automatic samplers may also be used to collect
samples within the first 30 minutes triggered by
the amount of rainfall, the depth of flow, flow
volume or time.
Commingling of parking lot runoff with
discharge associated with industrial activity.
The combined runoff must be sampled at the
discharge point as near as possible to the
receiving water or the parking lot drain inlet if
there is one.

Problem:
Solution:

Sampling in manholes.
Sample in manholes only when necessary, as
this requires training on confined space entry.

Problem:
Solution:

Run-on from other property.


If possible, estimate the volume of off-site runon contributions and off-site run-on sources of
pollutants to perform a mass balance calculation. Include this information in the permit
application. If this estimation is not possible,
provide a narrative discussion of the upstream
site (e.g., is it developed, if so the type of
facility, the types of pollutants that may be
present on the site, etc.).

Chapter 7 Storm Water Sampling

7.5.3.

Sample Type: Grab and Composite


Storm Water Samples
Because of the variable nature of storm water
flows during a rainfall event and different analytical considerations for certain pollutants, the
storm water regulations establish specific requirements for sample collection techniques. To
comply with storm water requirements, the sample
type (grab or composite) must be collected in
accordance with 40 CFR 122.21(g)(7) and 40 CFR
Part 136. Definitions of grab and composite storm
water samples are listed below.

Grab Sample. A grab sample is a discrete,


individual sample taken within a short period
of time, usually < 15 minutes. Analysis of
grab samples characterizes the quality of a
storm water discharge at the given time of the
discharge.
Composite Sample. A composite sample is a
mixed or combined sample that is formed by
combining a series of individual and discrete
samples of specific volumes at specified
intervals. Although these intervals can be
time-weighted or flow-weighted, the storm
water regulations require the collection of
flow-weighted composite samples. This
means that discrete aliquots or samples are
collected and combined in proportion to flow
volume rather than time. Composite samples
characterize the quality of a storm water
discharge over a longer time period, such as
the duration of a storm event. Flow-weighted
composite samples must be collected during
the first 3 hours of discharge or the entire
discharge (if it is < 3 hours) for industrial
facilities.
Storm water permits clearly specify which pollutants must be analyzed by grab sample and which
by composite sample. Although the requirements
in 40 CFR 122.21(g)(7) do not explicitly specify
either manual or automatic sampling techniques,
the approved analytical methods contained in 40
CFR Part 136 direct that grab samples must be
manually collected for certain pollutants. Table
7-2 provides a list of the typical pollutants that
are required for storm water permit compliance,
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and the type of sample (grab or composite) that


must be collected. The actual list of pollutants
for each facility will be included in the storm
water permit. The advantages and disadvantages
of using manual versus automatic sampling techniques for storm water samples are provided in
Table 7-3.
7.5.4.

Storm Water Sampling from Retention


Ponds
If storm water from a facility discharges after
flowing through a retention pond or other treatment system, sample as the storm water flows out
at the discharge point. Ponds may hold storm
water for a time before discharge begins. Sample
within the first hour, preferably 30 minutes from
when the pond begins to discharge.
Retention ponds with greater than a 24-hour
holding time for a representative storm event may
be sampled by grab sample. Composite sampling
may not be necessary. The rationale for this is
because the water is held for at least 24 hours, a
thorough mixing can occur within the pond.
Therefore, a single grab sample of the effluent
from the discharge of the pond may represent a

Chapter 7 Storm Water Sampling

composite of the storm water contained in the


pond. However, if the pond does not thoroughly
mix the discharge, thereby compositing the sample, then a regular grab and a composite sample
taken at multiple times should be taken at the
inflow to the pond. Since each pond will vary in
its capability to composite the water, permittees
must carefully evaluate whether the pond is thoroughly mixing the discharge.
Factors such as pond design and maintenance are
important in making this evaluation. For example, poor pond design, where the outfall and
inflow points are too closely positioned, can
cause short-circuiting and inadequate mixing. In
addition, poor maintenance may lead to excessive
re-suspension of any deposited silt and sediment
during heavy inflows.
Because of these factors, the permittee should
determine the best location to sample the pond
(e.g., at the outfall, at the outfall structure, or in
the pond) to ensure that a representative storm
water sample is taken. If adequate compositing
does not occur within the pond, the permittee
should conduct routine grab and flow-weighted
composite sampling.

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Table 7-2. Typical Storm Water Pollutants, Possible Analytical Methods, and Sample Collection
Techniques
Storm Water Pollutant
pH
Temperature
Oil and Grease
TSS
BOD5
COD
Nitrate and Nitrite Nitrogen
Ammonia Nitrogen
Fecal Coliform
Fecal Streptococcus
Total Phosphorous
Priority Metals
Total Cyanide
Total Phenolics
VOCs
SVOCs
Pesticides

Possible Analytical Method


Field measurement
Field measurement
EPA 1664
EPA 160
EPA 405
EPA 410
EPA 353
EPA 350
Standard Methods 9222
Standard Methods 9230
EPA 365
EPA 200, 200, 200, and 245 (Mercury
Only)
EPA 335
EPA 420
EPA 1624
EPA 1625
EPA 1657

Sample Technique
Grab
Grab
Grab
Flow-Weighted Composite
Flow-Weighted Composite
Flow-Weighted Composite
Flow-Weighted Composite
Flow-Weighted Composite
Grab
Grab
Flow-Weighted Composite
Flow-Weighted Composite
Flow-Weighted Composite
Flow-Weighted Composite
Grab
Flow-Weighted Composite
Flow-Weighted Composite

Table 7-3. Comparison of Manual and Automatic Sampling Techniques for Collection of
Storm Water Samples
Sampling Technique
Manual Grabs

Advantages
Appropriate for all pollutants
Minimum equipment required

Disadvantages
Labor intensive
Environment possibly dangerous to field personnel
May be difficult to get personnel and equipment to
the storm water outfall within the 30 minute
requirement
Potential for human error

Manual
Flow-Weighted
Composites (multiple grabs)

Appropriate for all pollutants


Minimum equipment required

Labor-intensive
Environment possibly dangerous to field personnel
Human error may have significant impact on
sample representativeness
Requires flow measurements taken during sampling

Automatic Grab
Samplers

Minimizes labor requirements


Reduced risk of human error
Reduced personnel exposure to unsafe
conditions
Sampling may be triggered remotely or
initiated according to present conditions

Samples collected for oil and grease (O&G) may


not be representative
Automatic samplers cannot collect samples for
VOCs analysis
Costly if numerous sampling sites require the
purchase of equipment
Requires equipment installation and maintenance
Requires operator training
May not be appropriate for pH and temperature
measurement
May not be appropriate for parameters with short
holding times (e.g., fecal streptococcus, fecal
coliform chlorine)

Chapter 7 Storm Water Sampling

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Sampling Technique

Advantages

Automatic
Flow-Weighted
Composite Samplers

Minimizes labor requirements


Reduced risk of human error
Reduced personnel exposure to unsafe
conditions
May eliminate the need for manual compositing of aliquots
Sampling may be triggered remotely or
initiated according to on-site conditions

7.6. Obtaining Flow Data


In addition to collecting samples of storm water
discharges, permittees must collect data characterizing the flow rate and flow volume for each storm
water discharge sampled. Flow rate is the quantity
of storm water discharged from an outfall per unit
of time. Total flow is a measure of the total volume
of storm water runoff discharged during a rain
event. Flow rate and volume either can be measured specifically or can be estimated, based on
rainfall measurements, velocities, and depth of
flows. To collect flow-weighted composite samples, flow rate data is necessary to combine proportional volumes of individually collected aliquots.
Permittees must also report the mass of pollutants
contained in storm water discharges. To determine
mass loadings of pollutants, applicants must measure both discharge flow rate and pollutant concentration. This section presents methods for obtaining
flow data.
7.6.1. Measuring Flow Rates
Flow rates for storm water discharges are most
accurately measured using primary flow measuring devices such as weirs, simple flumes, and
Palmer-Bowlus flumes. Weirs consist of a crest
located across the width of an open channel
(located at a right angle to the direction of the
flow). The flow of water is impeded, causing
water to overflow the crest. Weirs are inexpensive and particularly valuable in measuring flow
in natural or manmade swales because they are
easily installed in irregular shaped channels.
When flow exceeds the capacity of the weir and
Chapter 7 Storm Water Sampling

Disadvantages
Cross-contamination of aliquot if tubing/bottles
not properly washed
Not acceptable for VOCs sampling
Costly if numerous sampling sites require the
purchase of equipment
Requires equipment installation and maintenance,
may malfunction
Requires initial operator training
Requires accurate flow measurement equipment
tied to sampler
Cross-contamination of aliquot if tubing and
bottles not properly washed

water overtops the weir crest, flow depth actually


diminishes as the water approaches the weir and
flows cannot be measured accurately. Figure 7-4
is a diagram of a weir system showing the method
to calculate flow through a weir.
Flumes are structures that force water through a
narrow channel. They consist of a converging
section, a throat, and a diverging section. Figure 75 is a diagram of a flume and flow rates through the
flume. Flumes have fixed specifications relating to
geometric shape; they vary only in throat width.
Due to these geometric constraints, flumes may be
expensive to install. They typically are used in
permanent flow measurement points and are most
commonly placed in concrete-lined channels.
However, flumes can also be used in temporary
points. Flumes can provide accurate measurements
for a relatively wide range of flow rates.
Palmer-Bowlus flumes are also used for flow measurement at some facilities. Palmer-Bowlus flumes
are designed for installation in an existing circular
channel (e.g., a manhole channel) and are available
as portable measurement devices. Figure 7-6 is a
diagram of a Palmer-Bowlus flume flow measurement system. While Palmer-Bowlus flumes are
inexpensive, self cleaning, and easy to install, they
can only measure accurately over a narrow range of
flow rates. The flow from a Palmer-Bowlus flume
is calculated using the height between the floor of
the flume portion and the water level, not the total
head of the water level.
Where flow measurement devices are not already
installed, portable devices should be considered.
Page 7-15

DoD Environmental Field Sampling Handbook


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There are many permanent and portable types of


flow measurement devices available. Proper analysis of site discharge conditions must be conducted
prior to purchase and implementation of these
devices.

Figure 7-5. Flumes


Parshall Flume
Q = 0.338 H1.55
Q = 0.676 H1.55
Q = 0.992 H1.547
Q = 2.09 H1.55
Q = 3.07 H1.55
Q = 4 W H1 .522 W0. 26
1.6
Q = (3.6875 W + 2.5)H
Q = Flow rate
H = Depth of flow (Head)

Figure 7-4. Weirs


Q = 2.5 H2.5
Q = 1.443 H2.5
Q = 1.035 H2.5
Q = 0.676 H2.5
Q = 0.497 H2.5

V-Notch

(90)
(60)
(45)
(30)
(22)

Q = Flow Rate

(1 inch)
(2 inches)
(3 inches)
(6 inches)
(9 inches)
(1-8 feet)
(10-50 feet)

Flow

H = Depth of flow (Head)

Top View
W

Rectangular (without contractions)

Q = 3.33 L H1.5

Throat
Converging
Section

Side wall

Q = 3.33 (L 0.2 H)1.5

Rectangular (with contractions)

Diverging
Section
A

Side View

L
H

Source: Civil Engineering Reference Manual 5th Edition,


by Michael R. Lindeburg,
PE
.
.
With permission from the publisher, Professional Publications, Inc. Belmont, CA 1989
.

Contracted

Q = 3.367 b H1.5

Cipolleti (trapezoidal)

Figure 7-6. Palmer-Bowlus Flume


A

Source: Civil Engineering Reference Manual. 5th Edition, by Michael R. Lindeburg, PE,
with permission from the publisher, Professional Publications, Inc.,
Belmont, California, 1989.

Brace

B
Flow

A
PLAN

Trim to fit
As required

Palmer-Bowlus

Flow

Source: Wastewater Engineering: Treatment, Disposal, Reuse. 2nd Edition, Metcalf &
Eddy, Inc., with permission from the publisher, McGraw-Hill Book Co., New York, 1979.

Chapter 7 Storm Water Sampling

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7.7. Compliance Monitoring at Construction


Sites
CGPs may require that a visual inspection program be implemented to periodically evaluate the
integrity of the BMPs and visually observe and
note the condition of storm water leaving the
construction site. CGPs may also require that a
SAP be developed and conducted for pollutants
which:

Are not visually detectable in storm water


discharges
Are known to occur on the construction site
Could cause or contribute to an exceedance of
water quality objectives in the receiving water.
Pollutants that should be considered for inclusion
in the sampling and analysis strategy are those
identified during development of the SWPPP.
The CGP requires that the SWPPP identify a
strategy for conducting the sampling and analysis,
including the frequency and location(s) at which
sampling will be conducted. Sampling for nonvisibly detectable pollutants is usually required
under the following two conditions:

Visual inspections, currently required before,


during, and after storm events, indicate that
there has been a breach, malfunction, leakage,
or spill from a structural BMP that could result
in the discharge of pollutants in storm water
and the pollutants would not be visually
detectable
Storm water encounters soil amendments,
other exposed materials, or site contamination
that is discharged at a location off of the
construction site.
A sample of uncontaminated (background) storm
water from the site must be collected for comparison with the sample(s) collected from storm
water suspected of containing constructionrelated pollutants. The CGP may also state that
the SWPPP needs to describe the sampling procedure, location, and rationale for obtaining the
uncontaminated sample of storm water.

Chapter 7 Storm Water Sampling

7.7.1.

Known or Should Be Known


Pollutants at Construction Sites
Pollutants can be considered known or should
be known to occur on the construction site if
they are currently in use or are present because of
previous land uses. These may include the following materials:

Used in the construction activities


Stored on the construction site
Spilled during construction operations and not
cleaned up
Stored or used in a manner that presented the
potential for a release of the materials during
past land use activities
Spilled during previous land use activities and
not cleaned up
Applied to the soil as part of past land use
activities.
Construction material inventories and the project
SWPPP should provide adequate information on
materials currently in use or proposed for use on
the construction site. Dischargers should review
existing environmental and real estate documentation to determine the potential for pollutants to
exist on the construction site because of past land
use activities. Potential sources of information
for previously existing contamination and past
land uses include environmental assessments,
initial studies, environmental impact reports or
environmental impact statements prepared under
the requirements of NEPA, and Phase 1 assessments prepared for property transfers. In some
instances, the results of soil chemical analyses
may be available and can provide additional
information on potential contamination.
7.7.2.

Deciding When Sampling Is Required


at Construction Sites
All construction projects must ensure that proper
inspections are conducted throughout the duration
of the project to make sure that appropriate BMPs
have been implemented, are being maintained,
and are effective in preventing potential pollutants from coming in contact with storm water
and causing or contributing to an exceedance of
water quality objectives in the receiving waters.
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The frequency of sampling for non-visible pollutants must be determined based on the exposure
of pollutant sources. Runoff only needs to be
sampled when there is exposure of a pollutant
source to storm water that enters a storm drain or
surface water. Inspections of material storage
areas that identify a non-structural or structural
BMP failure that exposes potential non-visible
pollutants to storm water that runs off the construction site will trigger a requirement for sampling and analysis. If spills are cleaned up and
the contaminated material is isolated, eliminating
exposure to storm water runoff, then sampling is
not necessary. For instances when the potential
for previously existing contamination is identified, it may be appropriate to conduct screening
analysis during the first one or two storm events
of the season to determine if the potential contaminant is running off the construction site. Figure 7-7 provides a flow chart to help determine
when sampling and analysis is required.
7.7.3.

When Sampling and Analysis May Not


Be Required at Construction Sites
Sampling and analysis is typically not required
under the following conditions:

Where a construction project is selfcontained, meaning that the project generates


no runoff or any potential runoff discharges
containing pollutants, or pollutants can be
totally contained within the construction
project site without discharging to a water
body or storm drain system
Where construction materials and compounds
are kept or used so that they are not in contact
with storm water (e.g., in water-tight
containers, under a water-tight roof, inside a
building, etc.)
Where for specific pollutants, the BMPs
implemented at the construction site fully
contain the exposed pollutants (e.g., bermed
concrete washout area)
For building materials that are in their final
constructed form or are designed for exposure
(e.g., fence materials, support structures and
equipment that will remain exposed at the
completion of the project, etc.)
Chapter 7 Storm Water Sampling

Where pollutants may have been spilled or


released on site, but have been properly
cleaned up and storm water exposure has been
eliminated prior to a storm event
For stockpiles of construction materials for
which both cover and containment BMPs have
been properly implemented to protect them
from run-on and from contributing pollutants
to storm water runoff.
However, a contingency sampling strategy should
be prepared in the event of an incidental discharge. The SWPPP should also describe why
sampling and analysis is not expected to be
needed.
7.7.4.

When Sampling and Analysis May Be


Required at the Construction Site
Sampling and analysis is required when nonvisible pollutants have the potential to contact
storm water and run off the construction site into
a storm drainage system or water body. Examples of this situation follow:

Where construction materials and compounds


are stored or used such that they may
encounter storm water
For construction projects that utilize soil
amendments that can encounter storm water
runoff. (If independent test data are available
that demonstrate acceptable concentration
levels, sampling and analysis may not be
required. Contact the appropriate regulatory
authority to determine acceptable
concentration(s) of the material(s) in question.)
When a leak or spill occurs prior to a storm
event and is not fully contained and cleaned up
When a leak or spill occurs during a storm
event and cannot immediately be isolated or
cleaned up, and the possibility of an off-site
discharge exists
When, during regular inspections of stockpiles,
it is discovered that cover and containment
BMPs have been compromised and storm
water encounters the stockpiled materials
resulting in runoff discharging into a storm
drain system or water body

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When material storage BMPs have been


compromised, breached, or have failed. If
determined that sampling is needed, storm
water runoff samples must be collected
regardless of the time of year, status of the
construction site, or day of the week. Samples
should be collected during the first 3 hours of
runoff. Storm water inspections and sample
collections are required even during weekends
or holidays.
A list of potential pollutants must be developed
based on a review of potential sources from the
SWPPP. It should include construction related
materials, soil amendments, and historic contaminants. Identify from this list those pollutants that
are not visibly detectable. These constituents will
likely require sampling and analysis of runoff if
the materials are exposed to storm water. Consult
with an analytical laboratory or water quality
chemist to determine if there are field tests or
indicator parameters that can be used. Table 7-4
is a list of typical construction materials that
might cause non-visible contamination of runoff
if exposed to storm water.

affected by material storage, historic contamination or other exposed potential pollutants, and the
background runoff quality (i.e., uncontaminated
sample). Material storage may be confined to a
small area of the project site while historic contamination or exposed materials such as soil
amendments, may be widely spread throughout
the construction site. For this reason, the sampling locations identified for these two types of
potential pollutants may be different.
Samples must be collected at locations identified
in the SWPPP or areas identified by visual observations or inspections where there has been a
structural BMP failure or breach that can be
safely accessed. A location that is not affected by
material storage activities or by runoff from
material storage areas should be selected as a
background or reference sampling location for
collecting the uncontaminated runoff sample. For
a widely spread potential contaminant, sampling
locations may need to be selected at the perimeter
of the site, where storm water enters (unaffected
by site activities) and leaves (affected by site
activities).

7.7.5.

Deciding Where to Sample at a


Construction Site
Sampling locations must be identified that provide
information on both the runoff quality that is

Chapter 7 Storm Water Sampling

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Table 7-4. List of Common Potential Non-Visible Pollutants


Category

Potential Pollutant
Source

Field Indicator of
Pollutant Release

Laboratory Analysis

Line Flushing

Chlorinated water

Colorimetric kit

Residual chlorine

Portable Toilets

Bacteria, disinfectants

N/A

Total/fecal coliform

Concrete &
Masonry

Acid wash

pH meter

pH

Curing compounds

pH meter

pH, alkalinity, VOCs

Concrete rinse water

pH meter

pH

Resins

N/A

SVOCs

Thinners

N/A

VOCs

Paint strippers

N/A

VOCs

Solvents

N/A

VOCs

Adhesives

Phenols kit

Phenols, SVOCs

Sealants

N/A

SVOCs

Detergents

Colorimetric kit

Surfactants, phosphates

Bleaches

Colorimetric kit

Residual chlorine

Solvents

N/A

VOCs

Pesticides/herbicides

N/A

Check with analytical laboratory

Fertilizers

N/A

Nitrate, ammonia, phosphorous

Lime and gypsum

pH meter

Acidity/alkalinity

Aluminum sulfate,
sulfur

pH meter

TDS, alkalinity

Treated Wood

Copper, arsenic,
selenium

Metals test kits may be


available

Metals

Soil Amendments
& Dust Control

Lime, gypsum

pH meter

pH

Plant gums

N/A

BOD

Magnesium chloride

N/A

Alkalinity, TDS

Calcium chloride

N/A

Alkalinity, TDS

Natural brines

N/A

Alkalinity, TDS

Lignosulfonates

N/A

Alkalinity, TDS

Painting

Cleaning

Landscaping

Chapter 7 Storm Water Sampling

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Figure 7-7. Decision Diagram to Determine When Construction Storm Water Sampling is
Necessary
Start

Prepare SWPPP

Review Pollutants of Concern in


your SWPPP (per General Permit
Section A.5.b and A.5.c). Keep in
mind that Pollutants of Concern
include historic contaminants and
applied soil amendments that are
exposed to storm water runoff.

Are there
pollutants present that
are not visually
detectable in storm
water discharge?

No

Yes

No sampling and
analysis required for
these pollutants

No

Add pollutant to List of Potential


Pollutants to be Monitored

Is pollutant
stored in a water tight
container in a building
or under a water tight
roof?

Yes

Does visual
monitoring indicate
breach, malfunction,
leakage, or a spill, resulting in
release of pollutant so that it
could be discharged
in storm water
runoff?

No
Yes

Sampling and analysis is required:


1) at a discharge point that drains
the contact area;
2) at a reference (background) point;
3) within first two hours of
discharge; and
4) during daylight hours.

Chapter 7 Storm Water Sampling

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7.7.6.

Collection of Construction Storm


Water Samples
The conditions for collection of storm water
samples from construction sites are similar to
those outlined in Section 7.3.2 for industrial
sites. For instance, characteristics of the storm
event must be appropriate, e.g., accumulation
depth, representative storm, etc., and the sample
collection methods must adequately characterize
the discharge. On-site environmental personnel
responsible for storm water management at DoD
construction sites should consult their CGP or
the local permitting authority to determine specific sampling requirements.
The collection and handling of storm water
runoff samples requires special care to ensure
the integrity and validity of the samples. A
COC form must follow the sample from the
collection through the analysis process to document appropriate control of the sample prior to
analysis. Additional documentation to track
other information of interest, (e.g., field conditions or required field measurements) should be
recorded on a field tracking form. Every sample must be collected with care to ensure that
the sample is representative of the runoff being
tested, collected in the right kind of container,
preserved by chemical additives, and kept cold
in accordance with the test methods specifications, until delivered to an analytical laboratory.
Some types of samples have very short holding
times and must be analyzed before this holding
time is exceeded. Sample handling requirements and documentation form the basis of
your sampling QA program. More details
regarding QA planning are provided in Chapter
2 of this handbook.
Before starting any sampling program, contact
the analytical laboratory that will analyze the
storm water samples. Make sure to select a
laboratory that will provide the technical support that is needed, such as properly cleaned
and preserved sampling containers and COC
forms. Some laboratories can assist in identifying courier services available to transport samples to the laboratory. All these details need to
Chapter 7 Storm Water Sampling

be planned in advance of sample collection.


The analytical laboratory should also be consulted on requirements for additional samples to
be collected for QA/QC purposes.
Both field and/or analytical analysis methods
can be used to meet the permit requirements.
Field techniques have the advantage of providing immediate results. However, there are only
a limited number of analyses that can be conducted in the field. Some constituents (e.g.,
pH) can be evaluated in the field with special
equipment. Field samples must be collected
and analyzed according to the specifications of
the manufacturer of the sampling devices employed. Field equipment must be used by
trained staff, and the equipment must be calibrated and maintained according to the manufacturers specifications.
7.7.7.

Coupling Visual Observations with


Sampling Results
If visual inspection of non-structural and structural storm water BMPs used to contain nonvisible pollutants at a construction site indicates
that a BMP has failed or been compromised,
then field monitoring of the storm water for
non-visible pollutants is required. Of course,
any structural BMP that has been visually
inspected and found breached or compromised
should be immediately repaired or replaced.
The intent of conducting field monitoring for
non-visible pollutants is to obtain an immediate
indication if storm water that is discharging
from a site has been contaminated. An immediate indication of a polluted discharge requires
an immediate response in the form of back
tracking from the point of discharge to find the
source and take appropriate measures to prevent
a recurrence of a polluted discharge. If at all
feasible, the contaminated discharge should be
contained and prevented from being discharged
off site. After taking steps to correct the failed
non-structural or structural BMP, it is advisable
that field monitoring be conducted to verify that
pollutants are no longer in the storm water.

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7.7.8. Retention of Data


Results of field measurements and laboratory
analyses must be kept in the SWPPP, which is
required to be kept on the project site until the
Notice of Termination (NOT) is filed and approved by the appropriate control authority. It
is also recommended that field training logs,
COC forms, and other documentation relating
to sampling and analysis be kept with the
projects SWPPP. The GP requires that records
of all inspections, compliance certifications,
and noncompliance reporting must be retained
for a period of at least 3 years from the date
generated or after project completion, whichever is greater . Also note that continual monitoring of the non-structural and structural BMPs is
required until the NOT has been filed and approved.
7.8. Storm Water Sampling Equipment
Automated storm water sampling and flow
measurement equipment is available for a variety of situations. This equipment is designed to
operate with little or no operator attention,
eliminating the expense of mobilizing sampling
teams during storm events. Site environmental
personnel tasked with storm water sampling are
encouraged to discuss their specific site conditions with equipment vendors to be certain the
correct equipment is purchased.
7.9. Hazards and Safety Pre-Warnings
A project-specific HASP should be prepared for
each planned storm water sampling event.
Section 2.4 discusses preparation of projectspecific HASPs for all types of planned sampling activities. Since storm water sampling is
conducted during poor weather conditions, the
following specific health and safety issues
related to storm water sampling need to be
considered:

Hazardous weather conditions (e.g., wind,


lightning, flooding, etc.)
Sampling in confined spaces such as
manholes
Hazards associated with chemicals
Chapter 7 Storm Water Sampling

Biological hazards such as rodents and


snakes
Physical hazards (e.g., traffic, falling objects,
sharp edges, slippery footing, and the
potential for lifting injuries from opening or
removing access panels and manhole covers,
etc.).
It is essential that sampling personnel be aware
of these hazards. Sampling personnel should be
trained to evaluate potentially hazardous situations and develop ways for handling them.
Since sampling hazards can be life threatening,
safety must be the highest priority for all storm
water sampling personnel.
7.10. QA/QC
If the permit does not contain adequate sampling information, a SAP should be prepared for
collection of storm water samples at DoD industrial facilities and construction sites. Chapter 2
discusses development of SAPs. In general, the
storm water SAP will document the planned
activities for storm water data collection and will
provide a project-specific blueprint for obtaining
the storm water samples needed to verify compliance with the permit conditions. In general,
the SAP will document the following:

What samples are desired


How, where, and when the samples are to be
collected
Required sample size, containers, and
preservation
Required sampling documentation,
distribution, and storage
The turnaround times as required by the
permit or regulation
Where samples are to be sent for analysis
Analytical QA/QC samples
Sample disposal.
The SAP provides an in depth description of the
policies, organization, sampling activities, and
QC procedures necessary for achieving project
objectives. QC procedures are described in
detail to ensure a high level of quality in the
collection and analysis of the data and the
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handling of samples. Major elements in the


SAP include:

Title and approval page


Distribution list
Project organization
Project overview and schedule
Project quality objectives and measurement
performance criteria
Sample collection, documentation handling,
tracking and custody procedures
QC samples
Analytical requirements and procedures
Data management tasks
Assessment and response tasks.
The SAP should be prepared well in advance of
the planned sampling activities to allow for
approvals, laboratory coordination, and sampling personnel training and awareness.

7.11. Sampling Equipment List


Section 3.8 provides a generic sampling equipment list applicable to most sampling events.
The following list provides additional specific
equipment applicable to storm water sampling:

Sampling SOP
FLB/FN
Pen(s)
Containers
Preservatives
Labels
Markers
Coolers
Ice
Packing Material
Packaging Tape
COC form
Custody seals (if required)
Decontamination storage containers,
equipment, and materials
Personal safety equipment, safety test
equipment
Field screening or testing equipment,
standards, reagents, and SOP
Testing Field Forms or Logbooks.

Map of sampling location(s)

Chapter 7 Storm Water Sampling

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DoD Environmental Field Sampling Handbook


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Chapter 8. Groundwater Sampling


8.1. Purpose

8.3. Project Planning

This chapter provides procedures for obtaining


representative samples of groundwater.

This section provides an overview of the planning


process for conducting a groundwater sampling
program. Included in this section is a discussion
of sampling strategy, development of a sitespecific SAP, and QA considerations.

8.2. Scope
Groundwater monitoring wells, underground
injection wells, and industrial wells are the potential sources of groundwater samples. This chapter includes the minimum criteria to be followed
to obtain representative samples. Variations from
these criteria should be necessary only when
required by regulatory practices (e.g., statespecific requirements) or site historical data
gathering practices. Analytical data derived from
samples obtained in a way that does not follow
the documented sampling plan should not be
accepted. For construction and design of
groundwater monitoring wells, refer to ASTM
D5092-04, Standard Practice for Design and
Installation of Groundwater Monitoring Wells.
Figure 8-1 displays a diagram of a typical
groundwater monitoring well.
Figure 8-1. Diagram of a Typical Monitoring
Well

Source: Natural Resources Conservation Service.


Chapter 8 Groundwater Sampling

Before groundwater sampling begins, clear and


concise objectives must be developed regarding
the intent of the sampling. The objectives provide the framework for developing a sampling
strategy for the site and preparing the SAP. Some
common objectives of groundwater sampling
might include verifying that pollutants are not
migrating off site, defining the vertical and horizontal extent of pollutant concentrations from a
known source, or evaluating the progress of
groundwater remedial activities. Once the objectives are established, a sampling strategy can be
developed.
8.3.1. Sampling Strategy
The sampling strategy is designed around the
objectives and should utilize the conceptual site
model. The model takes into consideration historical site use, known or suspected pollutant
releases, and site geology and hydrogeology. The
conceptual site model is dynamic and is constantly revised as new information is collected and
processed. The model focuses on contaminant fate
and transport processes, the control of geologic
materials on the contaminant pathways (e.g.,
depositional environments, geologic structure, soil
characteristics), the types of contaminants present
(hydrophobic versus hydrophilic), and the
processes that influence the concentrations of
contaminants present such as dilution, biodegradation, and dispersion. More information on conceptual site models can be found in Chapter 2 of
this handbook.
8.3.2. Site-Specific SAP
Groundwater sampling should collect a representative sample of the current groundwater conditions over a known or specified volume of aquifer. Procedures that minimize disturbance to the
aquifer will yield the most representative
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groundwater samples. The development of a sitespecific SAP is the first step toward collecting a
representative groundwater sample. Each SAP is
an instruction manual for field personnel and
should be built around the objectives and sampling strategy. See Chapter 2 for a detailed discussion of SAP development applicable to all
sampling programs. The discussion below focuses on SAP development for groundwater sampling programs specifically.
The SAP should consider a variety of factors,
including site hydrogeology, the condition and
accessibility of monitoring wells, suspected
pollutants, DQOs, analytical methods and detection limits, the groundwater collection method,
sample handling procedures (e.g., filtration,
preservation requirements, COC), and safety.
The SAP cannot be implemented effectively if field
personnel do not understand its contents. Many
times the primary reason that groundwater sampling
events are problematic is that the person preparing
the SAP is not the person in the field. One method
that alleviates this problem is assigning a Sampling
Team Leader who is responsible for all activities in
the field. The Sampling Team Leader will work
closely with those individuals preparing the SAP to
understand fully the objectives of the project. The
Sampling Team Leader is responsible for all individuals in the field. If required, he or she also is
responsible for providing additional training to field
personnel before fieldwork begins.
8.3.3. QA
Groundwater monitoring programs encompass a
variety of information sources and include both
primary and secondary data collection. These
data sources are used to continuously update the
conceptual site model and allow Site Managers to
make decisions regarding further investigation,
additional monitoring, remediation alternatives,
or site closure.
The level of data quality for each groundwater
monitoring program, and many times for each
specific sampling event, depends on the intended
use of the data. For example, the level of QA/QC
needed for groundwater samples that are colChapter 8 Groundwater Sampling

lected on a monthly basis to monitor the progress


of remedial activities may be different from that
for groundwater samples collected because of an
enforcement action. It is important to remember,
regardless of the level of QA/QC for any
groundwater sampling, that sample integrity be
maintained during sample collection. Laboratory
analysis, no matter how sophisticated, is representative only if the sample supplied to the analyst has retained its integrity. During ongoing
groundwater monitoring studies, consistency of
sampling is crucial to the interpretation of the
data over the year or years.
To determine the level of quality required for
each groundwater sampling event, Site Managers
and those responsible for data integrity should
begin with a systematic planning process that
helps define the DQOs. The DQOs clarify the
study objective, define the most appropriate type
of data to collect, determine the most appropriate
conditions for data collection, and specify tolerable error limits on decisions that will be used as
the basis for establishing the quantity and quality
of data needed to support the decision. Detailed
information on QA/QC, including the systematic
planning process, development of DQOs, and
preparation of SAPs, is available in Chapter 2 of
this handbook.
QA/QC related specifically to groundwater monitoring programs can be categorized into the following four areas:
1. Use of secondary data for preparation of the
conceptual site model
2. Impacts of sampling equipment and well
construction materials on sample integrity
3. Equipment decontamination, and
4. Collection of QC samples.
8.3.3.1. Secondary Data
Secondary data are those data collected in addition to sampling data. For a groundwater sampling program, secondary data may include items
such as historical records regarding site use,
spills, and corrective actions on neighboring
properties; current and historical subsurface
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utility maps; locations of previous above-ground


and below-ground structures; possible disposal
areas; and areas containing fill materials or other
antidotal agents. These data aid the site manager
in selecting groundwater sampling locations or
determining possible pollutants.
For secondary data, acceptance criteria are used
in place of the measurement performance criteria
typically used for laboratory data. In general,
acceptance criteria are used to assess secondary
data adequacy and evaluate uncertainty in the
results derived from the use of secondary data
sources. For example, the Project Manager for
the groundwater monitoring program may require
interviews of former employees to validate the
location of disposal areas found on historical site
maps. In this case, the acceptance criteria are the
verbal confirmation of the disposal areas by the
former employees. The SAP for each groundwater monitoring project will explain the acceptance
criteria for determining which sources of data are
sufficient to support the project objectives.
8.3.3.2. Equipment Specifications for QC
The materials used for constructing groundwater
sampling equipment are critical to the collection
of valid monitoring data, particularly when volatile organic, pH-sensitive, or valence-reduced
chemical constituents are being evaluated. The
construction materials that come into contact with
the sample are as critical as the composition of
the laboratory sample containers. The recommended materials for bailers, pump parts, tubing,
other sampling devices, and associated apparatuses in decreasing order of preference are as follows: Teflon, stainless steel 316, stainless steel
304, polypropylene, linear polyethylene, polyvinyl chloride (PVC), Viton, and conventional
polyethylene.
Most regulatory programs require that bailers be
constructed of Teflon or stainless steel. Additionally, any other devices contacting the water to
be sampled should be constructed of Teflon or
stainless steel. Exceptions to this requirement
should be confirmed and approved by the regulatory program having project oversight authority.

Chapter 8 Groundwater Sampling

Tubing used in well evacuation may consist of


materials other than Teflon, but this tubing may
not be used for sample collection. Tubing should
be dedicated for use in each individual well for
that particular sampling event.
8.3.3.3. Equipment Decontamination
Decontamination of existing and new equipment
is required prior to use in the field. Section 8.5.3
describes decontamination procedures for various
types of groundwater sampling equipment. These
procedures must be followed to prevent crosscontamination between sites and within the site.
Equipment field blanks may be collected at the
start and end of the sampling event to determine
the cleanliness of the sampling devices and evaluate the cleaning techniques used in the field.
Decontamination procedures for all equipment
that contacts groundwater must be included in the
SAP.
8.3.3.4. QC Samples
In an attempt to identify external variables affecting groundwater sample integrity, a program of
QC blanks should be initiated. For volatile parameters, the QC blank sample program is a twotrack approach using both a trip and a field blank.
The trip blank acts as a check on potential contamination sources in the sample container, method
blank water (including preservative), and sample
transport and storage. The field blank acts as a
check on the cleanliness of the sampling equipment, potential atmospheric contamination, and
the effects of sampling procedures such as preservation on the analytes of interest. Complete
documentation on the sources of these materials
will assist with any problem solving.
Equipment field blanks may be collected at the
start and end of the sampling event to determine
the cleanliness of the sampling devices and evaluate the cleaning techniques used in the field.
Trip blanks, field blanks, and rinsate blanks
typically are prepared with metal-free and organic-free water purchased from a chemical supply
company or provided by the laboratory that is
performing chemical analyses on the groundwater
samples.
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Field duplicates or splits are collected in the field


in double the number of bottles required for the
regular sample. A duplicate sample is collected
concurrently, under comparable conditions, with
a first sample. Duplicate samples are QC samples
that are used to assess data repeatability based on
field conditions. Split samples are two or more
representative portions taken from one sample in
the field or in the laboratory and analyzed by
different analysts or laboratories. Split samples
are QC samples that are used to assess analytical
variability and comparability. Samples sent to
the same laboratory are duplicates, and samples
sent to a different laboratory are splits. Both
duplicate samples and split samples shall be field
homogenized and shipped to the laboratories as
blind samples. Duplicate samples provide a total
precision of field sampling precision and lab
analysis. Analytical data from these samples will
determine field precision (duplicate) or project
precision (split).
Field spikes are prepared in compliance with
permit or regulatory requirements. Field spikes
determine field accuracy or laboratory accuracy.
To prepare a field spike, a known amount of
contaminant is placed or spiked into the sample in
the field. Samples and spikes are handled in the
same manner. Field spikes help to assess analytical method performance and contaminant deterioration or degradation during sample handling,
transport, and analysis.
8.4. Hazards and Safety Precautions
The HASP should address all anticipated hazards
for each task. The following discussion contains
common (and commonly overlooked) hazards
associated with groundwater sampling activities.
Refer to Chapter 2 for specific hazard identification techniques and detailed control measures.
8.4.1. General Safety
Some of the general safety hazards associated
with groundwater sampling programs include the
following:

Moving sampling equipment and containers


across rough terrain either by hand or by
driving off road

Chapter 8 Groundwater Sampling

Conflicts with other uses of the area, such as


traffic conflicts when sampling next to roads
Sampling from deep sampling monitoring
wells or open holes using hand-held sampling
equipment.
8.4.2. Subsurface Hazards
Groundwater sampling, particularly monitoring
well installation, is an intrusive activity that could
expose sampling personnel to unidentified subsurface hazards, as discussed below.
8.4.2.1. Buried Munitions
If the probability of encountering buried munitions during the sampling program is moderate to
high, a RESS waiver from the relevant explosives
safety authority may be required prior to disturbing the site. In addition, a qualified explosives
safety expert will be required to accompany the
investigation team. See DoD TP18 for the minimum qualifications for unexploded ordnance
technicians and personnel. The site should be
checked by qualified personnel with groundpenetrating radar and/or metal detectors before
any samples are collected. Only trained and
certified personnel should handle or sample
explosive or suspected explosive materials.
8.4.2.2. Buried Utilities
The use of in situ groundwater sampling probes
to install monitoring wells can damage buried
utilities, including electrical and telephone lines
and gas, steam, water, and industrial pipelines.
Facility records should be reviewed carefully to
identify any buried utilities in the sampling area.
The site should be checked with groundpenetrating radar and/or metal detectors if there is
any question as to the presence of subsurface
utilities.
8.4.2.3. Toxic Chemicals
Collecting groundwater samples poses the risk of
exposure to hazardous chemicals. The following
major exposure scenarios should be evaluated.

Skin Contact with Contaminated Water.


Taking groundwater samples using hand-held
samplers usually results in the requirement to
handle wet equipment that can drip and splash.
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Decontamination of sampling equipment also


can result in splashes of contaminated water.
Field sampling and decontamination personnel
should wear waterproof rain gear or coated
Tyvek coveralls if there is a possibility of
contact with contaminated water.
Ingestion of Contaminated Water. Ingestion
can occur when food or drink is exposed to
contaminated water or is picked up with
contaminated gloves. Field personnel should
not eat, smoke, or chew gum or tobacco when
working with contaminated water. Drinking
water should be kept in closed squirt bottles or
should be stored outside the contaminated area.
Inhalation of Toxic Vapors. The exposure of
contaminated water to ambient air may generate
toxic vapors from the evaporation of VOCs. The
HASP should establish air-monitoring requirements for intrusive work and specify what air
monitoring equipment be used and the criteria
for the use of respirators. Either air-purifying
respirators or supplied-air respirators may be
required, depending on the toxicity of the chemicals present, the capabilities of the monitoring
equipment, and the warning properties of the
vapors.
Confined Space Hazards. In general, wells
more than 4 feet deep are considered confined
spaces. However, any well installed in
contaminated soil or water should be
considered a confined space, because
flammable vapors or toxic gases, including
hydrogen cyanide and hydrogen sulfide, could
accumulate. All applicable confined space
entry requirements should be imposed and
detailed in the HASP.
WARNING: Care should be taken to avoid breathing in
vapors that may escape from the well.

8.5. Field Preparation


The key to any successful field sampling program
is preparation. This section describes the preparations that should be made prior to personnel
entering the field to conduct a groundwater sampling event.

8.5.1. Access and Identification


Access to monitoring wells may be difficult, and
the wells themselves hard to locate in the field.
The Field Team Leader responsible for the
groundwater sampling should obtain recent well
location maps prior to the sampling event. In
addition, because access to some locations may
require permission from current owners or operators of the site, the Field Team Leader should
contact the site owner or operator in advance of
each sampling event to obtain access and inform
those individuals responsible for the site that
groundwater sampling is scheduled. Monitoring
wells usually have a friction cap or a screw cap
and should be locked. Therefore, keys to unlock
the wells and tools for removing caps often are
necessary.
If several monitoring wells must be sampled,
proper identification of each well is essential.
The well permit number or any other assigned
number should be known. If numbers are not
assigned, a precise field description of each well
location will avoid confusion of the sample results. When several monitoring wells of known
or suspected contamination will be sampled, the
least-contaminated well should be sampled first.
Subsequent samples then should be collected
from wells in an ascending order of contamination. Well head readings using PIDs or FIDs can
aid in determining the order in which wells
should be sampled by providing information on
contamination levels.
8.5.2. Sampling Equipment Selection
The equipment used for specific groundwater
sampling events can vary greatly, depending on
the following factors:

Chapter 8 Groundwater Sampling

Type of well
Depth of well
Diameter of well casing
Depth to water
Contaminants likely to be encountered
Analytes of interest
Length of open hole (bedrock well)
Type, slot size, and length of screen
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Expected recharge rate of well.


The equipment required for groundwater sampling generally falls into two categories: 1)
equipment used to evacuate water in the well
casing, i.e., well development, and 2) equipment
used to collect a discrete sample for analysis.
However, in some instances, the device used for
evacuation may be the same as that used for
sample collection.
8.5.2.1. Field Measurement Equipment
Prior to well evacuation, groundwater level measurements are made in each groundwater monitoring well. If either floating or settled organic
phases are expected in the groundwater, the
thickness of these phases also should be measured. The equipment typically used to measure
groundwater levels includes the following:

Electronic tape that signals to the user when


the water level is reached
A hydrocarbon interface probe affixed to an
electronic tape to measure the depth to either
the floating or the settled organic phase, and
the thickness of the phase.
8.5.2.2. Well Evacuation Equipment
Evacuation or purging of the water column in a
monitoring well is required prior to sample collection to remove the standing water column and
induce groundwater flow from the surrounding
formation into the well. One exception to this
standard procedure is if the objective of the sampling event is to determine the presence of dense
or light non-aqueous phase liquids or stagnant
water. The following types of pumps are available for well purging:

Suction lift pump/centrifugal pump


Portable submersible pump
Peristaltic pump
Air lift pump
Bladder pump (gas squeeze pump)
Packer pump
Gas piston pump
Gas displacement pump
Inertial pump.

Chapter 8 Groundwater Sampling

8.5.2.3. Sample Collection Equipment


The types of equipment available for groundwater
sample collection include the following:

Bottom fill bailer (single or double check


valve)
Peristaltic pump
Bladder pump
Packer pump
Inertial pump
Syringe sampler
Disposable equipment.
Site-specific sampling conditions will dictate the
optimal sampling equipment. Generally, sampling equipment that minimizes agitation, air
content, gas exchange, and depressurization is
preferred.
A list of additional sample collection equipment
is provided at the end of this chapter.
8.5.3.

Equipment Cleaning and


Decontamination
For each sampling event, all field measurement
and sampling equipment that will enter the well
must be cleaned prior to its entry. Field measurement equipment, such as water level indicators, should be cleaned in the following manner:

1. Wipe with a paper towel to remove visual


debris
2. Wash with tap water and a laboratory-grade
glassware detergent
3. Rinse with tap water
4. Perform an ASTM Type II water rinse.
Sampling equipment should be cleaned using
documented cleaning procedures. The sampling
equipment then should be wrapped in clean foil
and dedicated to a specific well for the days
sampling. The sampling equipment should remain wrapped in this manner until immediately
prior to use. Additionally, bailers and sample
bottles must be physically separated from pumps
and generators during transport and storage.
Pumps and equipment not amenable to precleaning should be field-cleaned using documented cleaning procedures. Down-hole devices
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such as water level indicators should not be


transported in a vehicle storing gasoline or gasoline powered equipment or other volatile contaminants such as degreasers, cleaning solvents,
and other volatile organics.

lowered into the well and remains for less than 1


minute. The wetted tape/stick gives the depth to
the top of the liquid and the color change section
indicates the depth to water. This procedure is
accurate to 0.02 feet.

8.6. Sampling Monitoring Wells

Wells with a non-aqueous phase liquid layer on


the surface pose a problem when measuring the
level of groundwater. A more accurate and easier
device to use is the interface probe. This probe
uses an optical sensor to determine if the probe is
in liquid, and a conductivity sensor to determine
if the probe is in water. When using this probe,
each phase can be measured independently. The
hydrocarbon/air interface reading should be taken
first, going down from the air to the hydrocarbon
surface to prevent any dripping hydrocarbons
from enhancing the thickness reading. The hydrocarbon/water reading is best taken going up
from the water to the hydrocarbon layer to prevent hydrocarbons from coating the conductivity
probe, which also would enhance the hydrocarbon thickness reading. Prior to taking the hydrocarbon/water reading, the probe should be lowered quickly through the hydrocarbon layer,
minimizing the contact time of the probe in the
hydrocarbon phase.

This section describes the procedures for sampling monitoring wells. It describes collection of
field measurements, well evacuation procedures,
and groundwater sampling procedures.
8.6.1.

Field Measurements

CAUTION: Be certain that the proper well is being


selected. The misidentification of a sampling point in the
field will result in data that may adversely affect important
decisions.

8.6.1.1. Physical Measurements


Once a well has been located and properly identified, note the field measurements listed below in the
FLB/FN.

Diameter of protective outer casing


Security and integrity of the well
Well number and well permit number
Inner diameter and construction material of
inner well casing
Total depth of well from the top of the inner
casing or surveyors mark, if present
(measured to 0.01 foot, or as appropriate).
8.6.1.2. Water Level Measurements
Well depths and water table depths can be determined using various measuring devices. A commonly used device is the electronic water level
indicator. This unit has a tape divided into incremental measurements of 0.01 feet and two
conductors forming a probe. When groundwater
is encountered, the circuit is completed causing a
signal (e.g., light, meter, or audible buzzer) to
activate. The depth to groundwater is then measured from this point to the reference mark on the
inner casing of the monitoring well.
Water indicator paste or gel acts as a colorimetric
test method when the paste comes into contact
with water. It is applied to the bottom few feet of
a measuring tape or rod. The tape or rod is then
Chapter 8 Groundwater Sampling

The key to accurate readings by any method is


proper collection of measurements from the same
survey point, preferably by the same person and
tape to avoid any procedural differences. Each
reading should be made three to four times. All
well measurements should be performed the same
day and prior to evacuation of any wells that
could influence groundwater elevations in the
area of investigation.
Water level elevation equipment should be properly decontaminated to avoid crosscontamination. In certain circumstances, sensitive components of an interface probe may be
compromised by the use of standard decontamination solvents. The manufacturers specifications for decontaminating interface probes should
be consulted before using any solvent.
For each water level measurement, the following
data should be recorded in the FLB/FN:

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Depth from casing top to water (recorded to


0.01 foot, or as appropriate)
Thickness of floating product, if any
Calculation of the linear feet of water in well by
subtracting the depth to water from the total depth
of well.
Note: Water levels should be obtained from all wells prior to
purging and sampling the first well, thus avoiding interference
problems. This procedure also allows personnel to determine
if any well is damaged or may pose a problem for sampling.

Using the physical measurements and water level


measurements, the amount of water within the
entire well casing can be calculated by multiplying the linear feet of water by the volume per foot
for the proper diameter casing.
Table 8-1. Volume of Water per Linear Foot in
Various Casing Sizes
Casing Diameter
(foot)

Gallons/Linear foot

2 inch (0.1667)

0.1632

4 inch (0.3333)

0.6528

6 inch (0.5000)

1.4688

8 inch (0.6667)

2.6112

10 inch (0.8333)

4.0800

12 inch (1.0000)

5.8752

Number of gallons = 5.8752 x C2 x H


where:

C = casing diameter in feet


H = height of water column in feet

8.6.1.3. Physio-Chemical Parameters


Information including specific conductance, pH,
temperature, DO, oxidation-reduction potential,
and turbidity may be recorded during well purging and before and after sample collection.
In some cases, additional physio-chemical analyses may be required to support the engineering
of future or current treatment processes. Samples
for these purposes are often collected for analysis
of common cations (Na+, K+, Ca+2, and Mg+2) and
anions (CO3-2, SO4-2, Cl-, and NO3-), dissolved
iron and manganese, TDS, TSS, TOC, and dissolved carbon. These are common and inexpensive analyses.
8.6.2. Well Development and Purging
Well development and well purging are two
similar operations that are conducted to ensure
that groundwater from a surrounding formation
flows into the monitoring well for sampling.
Each of these operations is discussed in the following subsections.

Example:
Total depth of well casing:
Depth to water:
Linear feet of water:
2-inch casing:

100 ft.
-20 ft.
80 ft.
x 0.1632

Amount of water in casing:

13 gal.

Table 8-1 above shows the volume of water per


linear foot of various casing sizes (inner diameter) of monitoring wells.
The amount of water in the casing then should be
multiplied by three to determine the minimum
volume to be purged from the well prior to sample collection. The total volume purged should
not exceed five times the amount of standing
water in the well.

Chapter 8 Groundwater Sampling

Alternatively, the following formula can be used


to determine the number of gallons in any diameter well:

8.6.2.1. Well Development


Well development typically is performed shortly
after construction of the monitoring well to ensure that free-flowing groundwater will enter the
monitoring well. Well development also is designed to provide removal of the following:

Drilling fluid residues remaining in the bore


hole or surrounding aquifer
Imported drilling water lost to the aquifer
during the drilling procedure
Groundwater in the bore hole or surrounding
aquifer that has been affected by the drilling
process or drilling or well construction
materials.
As well as:
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Restoration of the hydraulic properties of the


formation immediately surrounding the
monitoring well.
The length of time for groundwater conditions to
become representative (stabilization period) at
and near the monitoring well will vary depending
on site hydrogeologic conditions, drilling methods, and monitoring well development methods.
Groundwater flow velocities are typically less
than 1 foot per day, and natural flushing rates are
generally slow. If a monitoring well is drilled,
installed, and developed so that a 14-foot radius
around the well was left as unrepresentative, and
a natural groundwater flow rate was 1 foot per
day, it would take 14 days for representative
groundwater to reach the well. Sampling a monitoring well immediately after development generally will not be representative of the static
groundwater quality conditions at the horizontal
and vertical location of the monitoring well intake
interval. Therefore, all newly constructed and
developed monitoring wells should be allowed to
stabilize and equalize with the aquifer for a minimum of 2 weeks prior to sampling.
The installation and construction of monitoring
wells may alter the quality of groundwater in the
surrounding aquifer. Site-specific subsurface
conditions should be used to determine the appropriate well development techniques. Many
times, a combination of the techniques discussed
below will be necessary to produce a properly
developed monitoring well. Also discussed
below are certain outcomes inherent to well
development techniques that can be mitigated by
following the 14-day stabilization period:

High velocity air jetting, air lift, or surge block


development methods may introduce air into
the aquifer surrounding the monitoring well.
This air has the potential for altering groundwater quality, particularly for VOCs.
Over-pumping of a monitoring well for
development may draw groundwater to the
monitoring well from considerable distances.
This water may not be representative of the
horizontal and vertical location of the

Chapter 8 Groundwater Sampling

monitoring well, especially so for isotropic


and/or bedrock aquifers.
Organic drilling fluid residues and inorganic
residues of bentonite have been found to
remain in and near wells, even after proper
development. These residues have been found
to affect water quality, including the chemical
oxygen demand of groundwater samples, for
up to 100 days after completion of
development.
Non-aqueous phase liquid contaminants may
be pushed away or drawn to a monitoring well
location during development, depending on the
development method, resulting in nonrepresentative groundwater samples.
Suspended sediment not completely removed
by development and not allowed to settle out
may affect the quality of groundwater samples
obtained from the well. Therefore, a period of
time is required to allow a sand/gravel pack to
settle around a monitoring well screen.
Groundwater pollution investigations often base
expensive site-related investigatory and remedial
action decisions on initial (first sampling event
after development) groundwater sample analyses.
Therefore, before groundwater samples are collected, a complete understanding of the design,
construction, and hydrogeologic setting of the
monitoring well is necessary to interpret properly
any analytical results.
8.6.2.2. Well Purging
It is generally accepted that water in the well
casing is non-representative of the formation
water and should be purged prior to collection of
groundwater samples. Monitoring well purging is
a procedure that draws fresh groundwater from
the surrounding formation into the well immediately prior to sample collection. Wells are
purged to some extent for the following reasons:

The presence of the air interface at the top of


the water column results in an oxygen
concentration gradient with depth
Loss of volatiles up the water column
Leaching from or sorption to the casing or
filter pack
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Chemical changes due to clay seals or backfill


Surface infiltration.
Many methods may be used for well purging.
Not all are acceptable under all conditions. The
selection of a method is usually dictated by the
depth to water and local agency requirements.
The preferred and most commonly used methods
involve the use of a centrifugal or peristaltic
pump (when the depth to water is < 25 feet) and a
submersible pump (when the depth to water is >
25 feet).

should not be allowed to contact the ground or


any other potentially contaminated surfaces such
as gasoline pumps. If contact should occur, the
item should not be placed in the well or used for
evacuation.
The following information should be recorded in
the FLB/FN for each monitoring well sampled:

Note: The disposal or discharge of floating product or


hydrocarbons, and the discharge of highly contaminated
water, may require special purge water collection and
disposal procedures.

Before Purging
Date, time, and weather conditions
Well number and permit number
PID or FID reading taken from the well
immediately after the cap is removed
Presence and thickness of free product
pH, DO, temperature, and specific
conductivity
Total depth of well from the top of inner
casing or surveyors mark if present
Depth from the top of inner casing to the top of
screen
Depth from the top of inner casing to water
Estimated water volume in well.
After Purging
Start and end time purging
Purge method
Purge rate(s)
Total volume purged
pH, DO, temperature, and specific
conductivity.
After Sampling
Start and end time for sampling
pH, DO, temperature, and specific
conductivity
Sampling method.
Any field observations made during the groundwater sampling event (e.g., slow recharge, turbidity, odor, sheens, and PID or FID readings) also
should be reported.

Regardless of the purging procedure used, the


evacuation rate should not exceed that of well
development. Such an exceedance would cause a
redevelopment of the well, resulting in a turbid
sample. Cleaned equipment entering the well

Air-sensitive parameters such as DO, pH, temperature, and specific conductance are best analyzed with the use of a flow-through cell, eliminating sample exposure to air. However, monitoring of these air-sensitive parameters for well

It is important to ensure that the purging procedure or equipment does not cause crosscontamination from one well to the next. Therefore, the preferred method employs dedicated
tubing (new dedicated linear polyethylene ASTM
drinking water grade) and pumps. Because it
may not be practical to dedicate a pump to a
specific well, it is permissible to decontaminate
this equipment between wells. Methods for
decontamination should be specified in the sitespecific SAP.
Prior to purging, check the well for floating product. During purging, the pump intake or tubing
should be kept at a maximum distance of 6 feet
below the water level to prevent disturbance of
sediment on the bottom of the well. The pump
intake or tubing should be lowered as the water
level decreases to maintain this distance and
ensure sufficient distance from the air/water
interface. In instances where the total depth of
standing water in the well casing is less than 6
feet, begin purging near the top of the water
column and lower the tubing as stated above.
Following this procedure, Field Sampling Personnel should ensure that all static water is removed prior to sampling.

Chapter 8 Groundwater Sampling

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stability may not be a reliable indicator of when


to collect a representative sample. Therefore, if a
constant monitor is not used during well purging,
a sample should be collected within 2 hours after
3 5 volumes of water have been purged from
the well. The volume evacuated and the evacuation rate should be recorded after each purge and
sample event, and repeated for subsequent sampling events. This procedure should provide
consistent samples from each well.
Every reasonable effort should be made to keep
pumping rates low to avoid over-pumping or
pumping the well to dryness. Pump rates may be
adjusted and pumping times extended to remove
the required three to five well volumes. Sampling
should never occur more than 24 hours after
purging. To avoid altering the hydrogeologic
properties of the aquifer near the well, the evacuation rate of a monitoring well should not exceed that of the development of the well.
In some situations, evacuation of 3 5 volumes
may be impractical in wells with slow recoveries.
If a well has been pumped to near dryness at a
rate of less than 0.5 gallons per minute, the well
should be allowed to recover to a volume sufficient for sampling. If necessary, sampling within
the 2-hour limit may be exceeded to allow the
well to recover sufficiently for sampling. If a
well has been pumped to dryness, a minimum of
20 minutes of waiting time is required prior to
sampling, or follow regulatory requirements.
There are several reasons why the well should not
be pumped below the level at which the groundwater enters the well. In certain formations,
water entering the well at the top of the screened
area will fall into the pumped dry well. This
cascading effect may aerate the groundwater to be
sampled, thus resulting in the loss of VOCs.
Secondly, pumping to dryness can cause dehydration of the saturated zone; again, VOCs may be
lost due to aeration within this zone. Additionally, other contaminants may absorb to formation
materials where a dehydrated zone is created. As
a result, samples collected upon the recharge of a
well pumped to dryness may not correctly characterize groundwater quality.
Chapter 8 Groundwater Sampling

Another problem with excessive purging is the


entrainment of soils and other solids from the
formation into the well. Soils may contain either
metals or hydrophobic organic compounds that
become entrained into the well, resulting in an
overestimation of certain analytes. Soil particles
can be filtered from the sample; however, filtration may remove potentially mobile (contaminant-associated) constituents, resulting in artificially low concentrations. One method to reduce
entrainment of soil and other particulates into the
well is by using low-flow purging and sampling
techniques.
8.6.2.3. Low-Flow Sampling and Purging
The term low-flow refers to the pumping rate
during purging and sampling, which affects both
the velocity that is imparted to the formation pore
water in the immediate vicinity of the well screen,
and drawdown of the water level in the well.
When performed correctly, low-flow sampling
collects water from the formation surrounding the
screen and avoids collecting stagnant water from
any blank casing above the screen. Low-flow
purging and sampling reduces the effects of the
sampling on the system being sampled.
If little or no information about the groundwater
system is known, the pump intake may be set at
or near the middle of the well screen. However,
if available, knowledge of the well-specific hydrogeology, boring logs, well construction, and
well location relative to the lateral and vertical
contaminant distribution in the formation should
be considered when placing the pump intake.
The source of water moving into the screened
interval of the well under pumping conditions is
strongly influenced by the hydrogeology. In
wells where the screened interval intersects zones
of contrasting hydraulic conductivities, the composition under steady state purging conditions
will be flow-weighted in proportion to the hydraulic conductivity from any given point in the
flow field.
The objective is to pump in a manner that minimizes stress (drawdown) to the system to the
extent practical, while taking into account established site sampling objectives. The pumping
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rate must be low enough to minimize mobilization and entrainment of particulate matter that is
not mobile under non-pumping conditions. Typically, flow rates between 0.1 and 0.5 liters per
minute are used; however, the selection of an
appropriate flow rate is dependent on site-specific
hydrogeology. Water level drawdown provides
the best indication of the stress imparted by a
given flow rate for a given hydrological situation.
Measure the initial static water level, and then
monitor the water level of the well during purging
using either a continuous water-level measurement device such as a pressure transducer or
bubbler, or make periodic measurements (every 1
to 2 minutes) using an electric tape or similar
measuring device. If drawdown is rapid and
continuous, reduce the pumping rate until drawdown stabilizes. If drawdown is very slow or
imperceptible, the pumping rate can be increased.
When drawdown and water-quality indicator
parameters (e.g., conductivity, DO) have stabilized, sampling can begin in accordance with the
sites approved sampling and analysis plan.
In general, the advantages of low-flow purging
and sampling include the following:
More representative of the mobile load of
contaminants (dissolved and colloidassociated)
Minimal disturbance of the well, thereby
minimizing sampling artifacts
Less operator variability, and greater operator
control
Reduced stress on the formation (minimal
drawdown)
Less mixing of stagnant casing water with
formation water
Reduced need for filtration
Smaller purging volume, which decreases
waste disposal costs and sampling time
Better sample consistency, and reduced artificial sample variability.
Some disadvantages of low-flow purging include
the following:
Generally not suitable for use in low-yield
wells

Chapter 8 Groundwater Sampling

Higher initial capital costs for items like a


variable flow-rate pump or flow-through cell
Greater set-up and purging time in the field
Need to transport additional equipment to and
from the site
Increased training needs.
Even in low-yield wells, low-flow purging and
sampling may be more suitable than high-flow, or
purging to dryness and sampling by bailer or
pump as soon as the well recovers. Aeration of
the water column in a well caused by excessive
drawdown or pumping a well dry can significantly alter water quality, affecting redox-sensitive
metals, and causing increased turbidity and loss
of volatile constituents. If a well is evacuated to
dryness or below the well screen, sampling
records should document the event because sample integrity may be severely altered. For very
low-yield wells, or wells with severe turbidity
problems, passive or no-purge sampling methods
may be more appropriate and should be considered.
For additional information and more specific
procedures, see ASTM D 6771, Standard Practice for Low-Flow Purging and Sampling for
Wells and Devices Used for Groundwater Quality
Investigations.
8.6.3. Pumps
This section provides a discussion on various
pumps used for sampling groundwater.
8.6.3.1. Suction Lift Pumps/Centrifugal
Pumps
Suction lift pumps (e.g., diaphragm and centrifugal pumps) are used at the ground surface with
polyethylene tubing inserted into the well. They
are used to evacuate the well prior to sampling.
The tubing should be new, dedicated to a particular monitoring well, and equipped with a decontaminated foot check valve to avoid having aerated water from the pump spill back into the
well.
If a foot check valve is not used, care should be
taken to ensure that the entire pump impeller
chamber is drained after use and then thoroughly
decontaminated. Also, when removing tubing
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without a foot check valve after evacuation, the


pump should continue to operate to keep purged
water remaining in the tubing and pump chamber
from spilling back into the well.
The limitation posed by this type of pump is its
suction capability. Generally, the water level
must be within 25 feet of the ground surface.
Note: Take care to ensure that only ASTM Type II or better
quality water that is free from chlorine residual and potential contaminants is used to prime the centrifugal pump.
These pumps may be used only for well evacuation, not for
groundwater sampling.

8.6.3.2. Portable Submersible Pumps


When the depth to water is greater than 25 feet,
and if the diameter of the well casing will allow, a
portable submersible pump should be used. The
pump should be lowered carefully into the well,
trailing a discharge hose, electrical cables, and a
security cable constructed of approved material
(e.g., single-strand stainless steel or polyethylene).
The security cable should support all of the
weight of the pump. Hoses and cables can be
bundled together at 10-foot intervals with plastic
electricians ties or stainless steel clamps.
CAUTION: Duct or electrical tape must not be used at a
level that will be submerged into the water column. It is
important that the hose and electrical line be fed so they do
not jam between the pump and the casing. Similarly, the
hose and electrical line must be pulled up ahead of the
pump during removal.

Once the end of the purged line is fitted with a


gate valve in the closed position, the submersible
pump should be lowered to the appropriate depth.
The pump then can be turned on and the gate
valve adjusted to provide the correct flow rate.
During evacuation, it may be necessary to lower
the pump as the static groundwater level drops.
If a portable gasoline generator is used, it should
be placed downwind and at some distance away
from the well so fumes from the generator will
not affect sample quality. The generator should
only be operated during the purging process and
not during sample collection.
The pump should be fitted with dedicated tubing
for the discharge of evacuation water. As with
suction lift pumps, submersible pumps should be
Chapter 8 Groundwater Sampling

equipped with a check valve to avoid having


water from the pump spill back into the well. If
the same submersible pump is to be used for more
than one well, then the pump should be decontaminated between well locations to ensure that no
cross-contamination occurs.
Submersible pumps are susceptible to clogging.
Turbid groundwater or poorly developed monitoring wells are likely to impede the evacuation
process. Take care not to let the pump draw from
the bottom of the well where silts and sands may
be taken up by the pump.
8.6.3.3. Peristaltic Pumps
A peristaltic pump is a self-priming suction lift
pump used at the ground surface. It consists of a
rotor with ball bearing rollers. One end of dedicated tubing is inserted into the well. The other
end is attached to a flexible tube that has been
threaded around the rotor, out of the pump, and
connected to a discharge tube. The liquid moves
entirely within the sample tube, with no part of
the pump contacting the liquid. The bottom
length of tubing should be equipped with a foot
check valve to avoid having water from the pump
and tubing spill back into the well.
Use of a peristaltic pump for well evacuation is
limited to its suction capabilities. Generally, a
peristaltic pump cannot be used to evacuate wells
with a depth to water of greater than 25 feet. Due
to the volume present in large-diameter and highyield wells, peristaltic pumps are not recommended.
8.6.3.4. Air Lift Pumps
Air lift pumps generally are used for well development and not for well evacuation prior to sampling. If logistics dictate that air lift pumps are
the only alternative for evacuation, they should be
used only for wells screened below the water
table. Tubing connected to air lift pumps should
be placed above the well screen because air may
become trapped in the screen or filter pack.
Entrapped air can alter the oxidation-reduction
potential of the aquifer material around the well
bore, which can affect the chemical composition

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of groundwater samples. In addition, only oilfree compressors should be used.

pumps. Exposures to high-level contamination


may deteriorate the rubber with time.

8.6.3.5. Bladder Pumps (Gas Squeeze Pumps)


A bladder pump consists of a stainless steel cylindrical housing that encloses a flexible membrane. A screen is attached to filter any material
that can clog the check valves located above and
below the bladder. The pump works as follows:
water enters the membrane through the lower
check valve, and compressed gas is injected
through a separate line to the space between the
bladder and the pump housing. As the bladder is
squeezed, the water in the bladder closes the
lower check valve and flows through the upper
check valve. As the air pressure is released, the
upper check valve closes and water enters the
pump through the lower check valve. The compressed gas does not come into contact with the
sample water.

8.6.3.7. Gas Piston Pumps


The gas piston pump provides continuous sample
withdrawal at depths greater than possible with
most other methods. The pump consists of a
stainless steel alternating chamber between two
pistons. Pressurization of the alternating chamber
activates the pistons, which allows water to enter
during the suction stroke, and forces water to the
surface during the pressure stroke.

The bladder pump is used much like a portable


submersible pump, except that no electrical lines
are lowered into the well. The source of gas for
the bladder is either bottled gas or an on-site oilless air compressor. Disadvantages posed by
using the bladder pump include the large gas
volumes needed, especially for greater depths,
and the potential for bladder rupture and slow
evacuation rates.
The preferred material of construction for bladder
pumps and any tube, joint, or other fixture that
remains in contact with the groundwater is Teflon or stainless steel.
8.6.3.6. Packer Pumps
Packer pumps consist of two expandable bladders
that, when inflated, isolate a section of the well
bore between them. They deflate for vertical
movement within the well. The advantage of this
type of pump is that a smaller volume of water is
required to be evacuated prior to sampling. Also,
several zones within a single well can be sampled. The sampler must be sure the zone that is
being sampled and packed is isolated from the
other zones.
Packer pumps are constructed of rubber and can
be used with submersible, gas lift, and suction
Chapter 8 Groundwater Sampling

8.6.3.8. Gas Displacement Pumps


Gas displacement pumps work by using gas to
force water out of a discharge line. They consist
of a cylinder with a check valve and two lines, an
air supply line and a water discharge line, and a
connection to the top. As the pump is lowered
into the water, it fills by hydrostatic pressure.
When air pressure is applied, the check valve
seals and water is forced out of the discharge line.
When the air pressure is released, the pump
chamber fills and the cycle repeats.
8.6.3.9. Inertial Pumps
The inertial pump consists of a single tube or pipe
with a foot check valve at one end. The check
valve allows water to enter the pipe but stops it
from draining out.
The pump is operated by raising and lowering the
tube over a short distance with rapid strokes. The
movement causes the water inside the pump to
travel upward due to its inertia. The movement
can be accomplished manually or with a powered
unit.
The advantages of using an inertial pump are its
ease of operation and low cost. However, the
inertial pump has several disadvantages, which are
listed below.

Its manual operation is labor intensive,


although mechanical advantage devices are
available
The tubing and foot assembly must be
dedicated to a well
Use in slow-recharge wells may cause the
water level to drop significantly and result in
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aeration of the water column during purging of


the well. Conversely, the inertial pump device
can be overwhelmed in a rapidly recharging
well leading to insufficient evacuation of the
water column.
8.6.3.10. Hand Bailing Techniques
Hand bailers come in a variety of sizes and volumes to accommodate most well casing diameters; see Figure 8-2 for an illustration of a
Figure 8-2. Bottom Fill Bailer

sampled. The preferred apparatus is a Tefloncoated stainless steel cable attached to a lowgear-ratio winch, which is connected to a tripod
standing over the well. This apparatus is preferred because it provides the most reproducible
bailing method. If this apparatus is not available,
the bailer may be lowered by hand using a Teflon-coated stainless steel leader.
Note: Braided stainless steel cable is coated with manufacturing oils that make decontamination difficult. Therefore,
Teflon coated, stainless steel is required for the bailer
leader since it will come into contact with the groundwater.

Take care if using stainless steel cable clamps to


secure the leader to the bailer. The integrity of
the Teflon may be compromised by compression while tightening the clamps, thus exposing
the braided wire. All cut ends of leaders must
have an end cap to prevent exposure of the stainless steel wire.
8.6.4.

Groundwater Sampling Procedures


Using Monitoring Wells
After purging the required volume of water from
the well, sampling can begin. If the well is a
quick recharger, sampling of the well should
occur immediately after evacuation. In most
cases, the time lapse between evacuation and
sampling should not exceed 2 hours.
bottom fill bailer. Hand bailing may be conducted if no other method of evacuation can
accomplish the task and the procedure is specified
in the SAP. However, bailing is the least recommended procedure for well purging due to the
potential for aerating the well water or possibly
introducing contaminants during the bailing
procedure. Bailing is the least recommended
method of purging when samples are to be collected for VOC analysis. If hand bailing is the
method of evacuation, it must be performed with
a laboratory-cleaned and dedicated Teflon or
stainless steel bailer. An additional laboratorycleaned and dedicated bailer is required for sample collection.
The bailer should be lowered slowly into the well,
using care not to aerate the groundwater to be
Chapter 8 Groundwater Sampling

If several monitoring wells must be sampled,


proper identification of each well is essential.
The well permit number or any other assigned
number should be known. If numbers have not
been assigned, a precise field description of each
well location will avoid confusion of the sample
results. When several monitoring wells of known
or suspected contamination will be sampled, the
least-contaminated well should be sampled first.
Subsequent samples then should be collected
from wells in ascending order of contamination.
Well head readings using PIDs or FIDs can aid in
determining the order in which wells should be
sampled by providing information on contamination levels.
Field personnel should pay strict attention to
proper decontamination procedures during
groundwater sampling; see Section 8.3.3.3.
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A variety of techniques and equipment (including


several of the pumps discussed in Section 8.6.3)
can be used to collect groundwater samples, as
discussed in the following subsections. The order
in which samples should be collected from each
well, regardless of sampling device, is as follows:
1.
2.
3.
4.
5.
6.
7.

VOAs
Purgeable organic carbons
Purgeable organic halogens (POXs)
Total organic halogens (TOXs)
TOC
Base neutrals/acid extractables
Oil and grease/total petroleum hydrocarbons
(O&G/TPH)
8. PCBs/pesticides
9. Total metals
10. Dissolved metals
11. Phenols
12. Cyanide
13. Sulfate and chloride
14. Turbidity
15. Nitrate and ammonia
16. Preserved inorganics
17. Radionuclides
18. Non-preserved inorganics
19. Bacteria.
This collection order takes into consideration the
volatilization sensitivity of groundwater samples.
Additional information on the order of sample
collection can be found in RCRA and the
Groundwater Monitoring Technical Enforcement
Guidance Document, September 1986.
8.6.5.

Overview of Passive Groundwater


Sampling in Monitor Wells
Passive groundwater sampling, sometimes called
no-purge sampling, employs devices and techniques to obtain quantitative information about
the concentrations of analytes of interest from a
groundwater monitoring well under ambient flow
conditions. The original suggested groundwater
application was for long-term monitoring at wellcharacterized sites (Vroblesky, 2001); however,
Chapter 8 Groundwater Sampling

the depth-specific nature and other characteristics


of passive samples also can make them very
useful for site characterization.
Passive samplers rely on the natural movement of
groundwater through the screened interval of a
monitor well to sample groundwater from the
adjacent aquifer. In a properly constructed and
developed monitor well, water in the screened
interval is constantly replaced by water from the
adjacent aquifer. The screened or open interval
of a well does not contain stagnant water, but
rather is in constant hydraulic communication
with the aquifer. The rate of exchange is driven
by the natural gradient of the groundwater system, and depends on the magnitude of the gradient and hydraulic conductivity of the aquifer.
The well screen and sand pack of a properly
designed well have a combined hydraulic conductivity greater than that of the aquifer materials,
and thus provide a preferential path that concentrates flow from the surrounding aquifer through
the well bore across the screened interval.
Groundwater flux through the screened interval
typically is greater than flow through the immediately adjacent aquifer.
Passive samplers typically are deployed on a
weighted line at a specifically chosen depth within the saturated portion of the screened or open
interval of a well. Care must be taken to ensure
that the sampler is placed at the selected depth
within the screened interval, and that the entire
sampling device remains submerged for the entire
deployment period.
In contrast to samples collected using a pump or
conventional rigid bailer, passive sampling has
negligible effect on the ambient flow in a well,
and does not alter the natural steady state conditions of the water column being sampled. Induced flow, even at low-flow rates (i.e., 200
500 mL/minute) may change conditions in the
water column, and artificially elevate turbidity by
mobilizing particles that are immobile under
laminar flow in the aquifer.

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8.6.5.1. Comparison of Passive Samples to


Pumped Samples
Passive and pumped sample collection methods
each have specific characteristics that should be
considered when selecting a sampling method,
and when analyzing groundwater analytical data.
Passive samplers collect depth-specific samples
representing a very limited depth interval (typically not more than 1 to 2 feet) of the water column in the well. They represent only the water to
which the sampler is exposed under ambient flow
conditions. Because passive sampling does not
affect flow through the well screen by pumping,
purging, or otherwise mixing the water column,
passive samples represent water from a confidently known, specific depth interval in the water
column.
Under ambient flow, water in the sampled interval typically is dominated by horizontal movement of water across the well screen, yielding a
sample that is representative of water at that
depth interval in the adjacent aquifer. However,
various degrees of well-specific vertical mixing
are present in the screened intervals of many
wells under ambient flow. In some wells, this inwell mixing obscures the details of analyte stratification in the aquifer, though in other wells,
contaminant stratification in the aquifer is clearly
present in the water column of the screened interval. Passive samplers have revealed vertical
concentration gradients in the well water column
over intervals as short as three feet. If the
screened interval intersects zones of different
pressure head, vertical flow through the well will
result. Water in the sampled interval will be
biased toward that from the zone of higher head.
In wells having a screened interval greater than 5
to 10 feet, obtaining a synoptic vertical profile of
concentration by spacing multiple passive samplers in vertical series should be considered for
the initial passive sampling event (Vroblesky,
2001a; ITRC, 2004). If stratified, the interval of
highest concentration can be monitored subsequently using a single sampler.
Pumped samples, both low-flow and high-volume
purge, collect a flow-weighted sample biased
Chapter 8 Groundwater Sampling

toward any zones of higher conductivity intersected by, or adjacent above or below the
screened interval. Also, flow induced by pumping, even at low-flow rates, can mobilize and
suspend solids that are immobile under ambient
laminar flow conditions in the aquifer, thereby
artificially elevating turbidity. This can result in
measured concentrations being affected by the
sampling process, particularly for metals. Vertical flow through the well caused by the screen
intersecting zones of different head also can bias
the representativeness of low-flow samples, as
well as that of passive samples, particularly if net
vertical flow through the well bore exceeds the
purge rate (sampled water will be biased toward
the source of flow). Side-by-side comparisons
and historical data show that concentration results
obtained by low-flow sampling most often are
very similar to concentration results obtained by
passive sampling (ITRC, 2007). Understanding
differences that may be observed often can provide valuable insight into contaminant distribution and hydrologic characteristics of a site.
8.6.5.2. Characteristics of Passive Samples
Passive samplers:

Represent a short, discrete interval of the water


column in the screened interval of a well
Can provide a vertical concentration gradient
profile of the water column and identify
whether contaminant stratification is present in
the well
Improve consistency of monitoring data over
time by reducing the number of variables in
sample collection such as pump intake depth,
adequate duration of low-flow purging, pumping rate, etc.
Eliminate or minimize turbidity
Greatly reduce field equipment needs thereby
facilitating sampling where access is difficult,
or where discretion is desired
Eliminate purge-water production, and costs
for its handling and disposal
Can be deployed in most monitor wells (i.e., 1inch diameter or greater)
Have no practical depth limit

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Allow rapid field sample collection; no time is


needed for purging or set up of equipment
With few exceptions, can remain deployed in a
well for up to a year without loss of integrity,
allowing the retrieval of a sample and replacement of the sampler for the next round of
sampling during a single site visit.
Some of these characteristics can be either an
advantage or a disadvantage, depending on sampling objectives. Many of these characteristics
serve to substantially reduce field labor and
equipment cost, particularly for long-term monitoring programs. Field sampling cost reduction in
long-term monitoring programs is typically between 40 and 70 percent (ITRC, 2004; ITRC
2007).
8.6.5.3. Limitations of Passive Sampling
Passive samplers:

Require time for equilibration (typically up to


two weeks)
Are inappropriate for sampling where the
objective is to determine water quality from a
well under pumping conditions (e.g., a drinking water production well)
Provide limited sample volume, although
minimum sample volumes actually required
for a single analysis by many common analytical methods are often substantially less than
those routinely requested by the laboratory
(see ITRC, 2007, Appendix A).
8.6.5.4. Types of Passive Samplers
Passive groundwater samplers can be grouped
logically into three types, based on the operating
mechanism.
Diffusion-based Samplers. Rely on diffusion of
analytes from the well water into a sampler made
of a semi-permeable membrane material, initially
filled with deionized, analyte-free water. When
deployed to a specific depth in a well, analyte
concentrations in the sampler reach and maintain
equilibrium with concentrations in the water to
which they are exposed. The time required for
equilibration depends primarily on properties of
the membrane material, the diffusive characteristics of each analyte, and the temperature of the
Chapter 8 Groundwater Sampling

groundwater. The appropriate period of deployment also considers the time required for well
flow dynamics and ambient conditions to restabilize from placement of the sampler or other
disturbance. The rule of thumb is that a 14-day
deployment period is ample for most types of
diffusion samplers, analytes, and hydrologic
conditions (ITRC, 2004; ITRC, 2007). Because
analytes always diffuse across the membrane
from higher to lower concentration, the samplers
maintain equilibrium concentrations and track
changes in concentration in the well water (within
the equilibration time lag period) regardless of
how long the sampler was deployed in the well.
The very small pore sizes of diffusion sampler
membrane materials eliminate turbidity, thus
diffusion samplers represent only the truly
aqueous (dissolved) concentrations of analytes.
Polyethylene Diffusion Bag (PDB) Sampler.
(Vroblesky and Hyde, 1997; Vroblesky, 2001;
ITRC, 2004) was the first diffusion sampler to
become widely known for sampling groundwater.
PDBs are constructed of low-density polyethylene tubing of 4 mil thickness, having a pore size
of about 10 angstroms. They are appropriate for
sampling only hydrophobic (low water solubility)
VOCs, chlorinated solvents, and short chain
aliphatic hydrocarbons (up to about C10). The
hydrophobic nature of the polyethylene membrane makes PDBs inappropriate to sample for
analytes that are highly soluble in water (e.g.,
ketones, alcohols, etc.) or dissolved ionic species
(e.g., metal cations, anions). Tables listing many
field- and laboratory-tested analytes are found in
Vroblesky (2001a), Vroblesky and Campbell
(2001), ITRC (2004), and ITRC (2006).
Regenerated Cellulose Dialysis Membrane
Sampler. (Imbrigiotta and others, 2007) is similar in concept to the PDB, but uses a hydrophilic
cellulose membrane. The dialysis membrane
sampler was developed and demonstrated by
researchers at the US Geological Survey (Ehlke
and others, 2004) to provide a passive diffusiontype sampler appropriate for inorganic as well as
organic analytes. It has been demonstrated as
suitable for sampling dissolved concentrations of
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major cations and anions, most trace metals, all


analytes on the EPA Method 8260B list, semivolatile organic compounds, many explosives,
total dissolved solids, electrical conductance,
dissolved organic carbon, and dissolved gases.
Field and laboratory test results from dialysis
membrane samplers for many analytes are listed
in ITRC (2006; Tables 4-1 and 4-2). The pore
size of about 18 Angstroms excludes all suspended colloidal size particles, and organic molecules >~8000 Daltons. Field-ready dialysis samplers are not currently commercially available,
but can be constructed easily and economically
from the component materials. One potential
disadvantage of the dialysis sampler is that the
cellulose membrane is subject to biodegradation,
typically losing integrity in about 3 to 4 weeks in
most wells, and thus cannot be deployed for
extended periods (e.g., between quarterly longterm monitoring events).
Water from all equilibrium-type diffusion samplers should be transferred immediately upon
retrieval to appropriate laboratory containers for
transport and storage to minimize analyte loss,
particularly if volatile compounds are of interest.
Because diffusion through the membrane is reversible, VOC losses or other changes begin
occurring as soon as the sampler is removed from
the intended sampling location.
Whole-water grab samplers obtain an instantaneous sample of the water from a specific depth in
the water column of a well (ITRC, 2007).
Whole-water Grab Sampling Devices. Are
among the oldest groundwater sampling devices
(e.g., rigid bailer). However, recent improvements in design and sampling methods provide
samples from a specifically designated and confidently known depth in the water column, and
recommend an equilibration period of several
days to two weeks (ITRC, 2007) for both the well
and sampler to reach equilibrium with ambient
conditions before sample collection. Equilibration avoids analyte loss from the sample to sampling equipment, which can be significant, and
allows elevated turbidity and effects of sampler
placement or other disturbance to dissipate before
Chapter 8 Groundwater Sampling

sample collection. The sample is collected immediately prior to, or as a result of sampler retrieval. Properly collected whole-water grab
samples capture suspended particles that are
naturally mobile in the aquifer under ambient
laminar flow conditions, but do not have elevated
turbidity resulting from the sampling activity.
One of the more recently developed devices seals
the sample in situ at the sampling point in containers (e.g., 40-mL VOA vials or other containers) that can be placed directly into auto-samplers
at the laboratory, thus eliminating all exposure of
the sample to air or other influences. Sample
transfer can cause loss of VOC analytes, and
exposure to air can cause changes in oxidationreduction potential affecting redox-sensitive
metal concentrations.
Accumulationtype Samplers. Rely on both
diffusion and adsorption of analytes. Analytes
diffuse through a semi-permeable membrane and
are accumulated onto an adsorbent medium within the sampler. Both the diffusion membrane and
adsorbent material must be appropriate for the
analyte(s) of interest. The total analyte mass
accumulated on the adsorbent medium over the
entire deployment period is measured. Accumulation samplers have been used to sample surface
water (e.g., bioaccumulation studies) for several
decades (e.g., the SPMD, Polar Organic Chemical
Integrative Sampler (POCIS)) (ITRC, 2006;
Verreydt, 2010), and for air and soil vapor studies
(ITRC, 2006). More recently the methodology
has been applied to determine VOC concentrations in groundwater wells using the Gore
Module (ITRC, 2007). An average accumulation
rate over the deployment period is easily calculated, but estimates of concentration in the medium being sampled depend on a significant
number and range of analyte-specific, samplerspecific, and environmental variables (e.g., membrane and analyte diffusion properties, adsorbent
uptake rate, temperature, pressure, etc.). Proprietary empirical data for the Gore Module is used to
infer VOC concentrations in groundwater. Accumulation samplers have a particular advantage
in that the deployment period can be extended to
concentrate analyte mass and detect analytes
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present in the environment at concentrations too


low to be detected by other sampling methods.
Tables listing media and common analytes addressed by many passive sampling devices mentioned above, advantages and limitations specific
to each type of device, as well as summary of the
availability and cost of each type of passive
device are found in ITRC (2007, Tables 14-1, 142, 14-3), and in Verreydt and others (2010).

Vroblesky, D.A. (2001a). Users Guide for Polyethylene-Based Passive Diffusion Bag Samplers
to Obtain Volatile Organic Compound Concentrations in Wells, Part 1: Deployment, Recovery,
Data Interpretation, and Quality Control and
Assurance, U.S. Geological Survey Water Resources Investigations Report 01-4060.

8.6.5.5. References for Passive Sampling


For more information on passive sampling, see
the following references:

Vroblesky, D.A., 2001b, Users Guide for Polyethylene-Based Passive Diffusion Bag Samplers to
Obtain Volatile Organic Compound Concentrations in Wells, Part 2: Field Tests, U.S. Geological Survey Water Resources Investigations Report 01-4061.

Ehlke, T.A., Imbrigiotta, T.E., and Dale, J.M.,


2004, Laboratory Comparison of Polyethylene
and Dialysis Membrane Diffusion Samplers,
Groundwater Monitoring & Remediation,
24(1):53-59

Vroblesky, D.A., and Campbell, T.R., 2001,


Equilibration Times, Stability, and Compound
Selectivity of Diffusion Samplers for Collection of
Groundwater VOC Concentrations, Advances in
Environmental Research, 5:1-12.

Imbrigiotta, T.E., Trotsky, J.S, and Place, M.,


2007, Demonstration and Validation of a Regenerated-cellulose Dialysis Membrane Diffusion
Sampler for Monitoring Groundwater Quality
and Remediation Progress at DoD Sites, Final
Technical Report ESTCP Project ER-0313.

Vroblesky, D.A. and Hyde, W.T., 1997, Diffusion


Samplers as an Inexpensive Approach to Monitoring VOCs in Groundwater, Groundwater
Monitoring and Remediation, 17:177-184.

ITRC (Interstate Technology & Regulatory


Council), 2004, Technical and Regulatory Guidance for Using Polyethylene Diffusion Bag Samplers to Monitor Volatile Organic Compounds in
Groundwater, ITRC Technical and Regulatory
Guidance, Report DSP-3, February, 2004.
ITRC (Interstate Technology & Regulatory
Council), 2006, Technology Overview of Passive
Sampler Technologies, Diffusion/Passive Sampler Team, Report DSP-4.
ITRC (Interstate Technology & Regulatory
Council), 2007, Protocol for Use of Five Passive
Samplers to Sample for a Variety of Contaminants in Groundwater, ITRC Technical and
Regulatory Guidance, Report DSP-5.
Verreydt, G., Bronders, J., Van Keer, I., Diels, L.,
and Vanderauwera, P., 2010, Passive Samplers
for Monitoring VOCs in Groundwater and the
Prospects Related to Mass Flux Measurements,
Goundwater Monitoring & Remediation,
30(2):114-126.
Chapter 8 Groundwater Sampling

8.7. In Situ Groundwater Sampling Using


Probes
This section provides a description of the equipment and techniques that can be used to collect
samples using probes rather than monitoring
wells. It is important to check with state environmental agencies to determine if groundwater
data collected from probes can be used for decision-making purposes or site closure.
A relatively new development in groundwater
sampling technology has been the design of in
situ sampling probes, which allow for the collection of groundwater samples without the installation of permanent wells. A hydropunch operates
in conjunction with conventional cone penetrometer rigs. The category of in situ sampling
probes also includes a variety of driven probes,
which can be retrieved after sampling or left in
place as permanent sampling points. These devices often are used during the preliminary site
characterization stage or where only a shallow
water table is to be sampled. The portable in situ

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samplers can be valuable in determining the best


location for permanent monitoring wells.
CAUTION: Not all states accept groundwater data collected with probes. Site Managers should consult state
environmental agencies when developing the SAP to determine how groundwater data from probes can be used.

8.7.1. In situ Well Installation


Direct push technology (DPT) is an example of
an in situ groundwater sampling tool that can be
used to install point-in-time groundwater sampling probes and wells. A description of some
DPT technologies is provided below.
8.7.1.1. Point-in-Time Groundwater
Sampling Probes
Point-in-time probes, also referred to as temporary samplers or grab samplers, are used to
collect samples rapidly to define groundwater
conditions during one sampling event. They are
usually less than 2 inches in outside diameter
(OD) and are generally constructed of steel or
stainless steel. Direct-push methods (percussion
or static weight) are used to advance point-intime samplers below the static water level in
unconsolidated formations. Generally, groundwater flows into the sampler from an exposed
screen under ambient hydrostatic pressure.
Groundwater may be collected from the sampler
using bailers or pumps, or the sampler may be
retracted to the surface to obtain the water sample. Once sampling is completed, these devices
are removed and the boring should be abandoned
in accordance with local regulations.
8.7.1.2. DPT-Installed Groundwater
Monitoring Wells
DPT-installed monitoring wells permit short-term
or long-term monitoring of groundwater. They
are usually 2 inches in diameter or less and constructed of PVC or stainless steel. Because monitoring wells are installed for periods of several
months to several years, the annulus of the boring
around the well casing is usually sealed to prevent migration of contaminants into the aquifer.
Surface protection is required to prevent tampering with the well. A slotted or screened section
permits groundwater to flow into the well under
Chapter 8 Groundwater Sampling

ambient hydrostatic pressure. Groundwater may


be collected from monitoring wells using bailers,
various pumps, or passive sampling devices.
8.7.2. Point-in-Time Sampling
Ideally, DPT point-in-time and monitoring well
groundwater sampling equipment should be used
together to maximize their effectiveness. Pointin-time sampling techniques generally are better
for identifying plume boundaries, hot spots,
preferred pathways, or other monitoring points of
interest.
A variety of point-in-time groundwater sampling
tools are available for site characterization, including the following:

Sealed-screen samplers
Multi-level samplers (or vertical profilers)
Open-hole samplers.
With these tools, the time needed to retrieve the
sample will vary according to the hydraulic conductivity of the sampling zone. In general, sampling within coarse-grained sediments takes
minutes, while sampling within fine-grained
sediments can take several hours or more. In
situations where slow recharge inhibits the timely
collection of groundwater samples, the sampler
may be left in place to recharge while the DPT rig
is moved to a new sampling location.
8.7.2.1. Sealed-Screen Samplers
Sealed-screen samplers typically consist of a
short (6 inch 3-foot) screen nested within a
sealed, watertight tool body. Because the screen
is not exposed to the formation as the sampler is
advanced into the subsurface, the screen does not
become plugged or damaged. In addition, the
potential for cross-contamination is greatly reduced and a true depth-discrete sample that is
representative of the target sampling zone can be
collected. The sample volume collected with
some sealed-screen samplers is limited by the
volume of the sample chamber.
To collect the sample, the sealed-screen sampler
is advanced to the target sampling depth, and the
protective outer rod is retracted, exposing the
screen to groundwater. Groundwater flows
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through the screen and into the drive rods or


sample chamber under the hydraulic head conditions that exist at that depth. O-ring seals placed
between the drive tip and the tool body help
ensure the sampler is watertight as it is driven to
the target sampling interval. The integrity of the
seal often can be checked by lowering an electronic water level indicator into the sampler prior
to retracting the protective outer rod.
8.7.2.2. Multi-level Samplers
Multi-level samplers, most of which are exposedscreen samplers, are DPT equipment capable of
collecting groundwater samples at multiple intervals as the sampling tool is advanced. One benefit is they do not have to be withdrawn for sample
collection or decontamination. The terminal end
of a typical multi-level sampling tool has a 6 inch
3 foot-long screen made up of fine mesh, narrow slots, or small holes. The screen remains
open to formation materials and water while the
tool is advanced. Samples are collected either
continuously or periodically as the tool is advanced to vertically profile groundwater chemistry and aqueous-phase contaminant distribution.
Multi-level samplers can be used to measure
water levels at discrete intervals within moderateto high-yield formations to assist in defining
vertical head distribution and gradient. Additionally, some of these tools can be used to conduct
hydraulic tests at specific intervals to characterize
the hydraulic conductivity in formation materials
and identify possible preferential flow pathways
and barriers to flow.
8.7.2.3. Open-hole Sampling Methods
Open-hole sampling is conducted by advancing
drive rods with a drive point to the desired sampling depth. Upon reaching the sampling depth,
the rods are withdrawn slightly, which separates
them from the drive tip and allows water to enter
the rods. The water can be sampled by lowering
a bailer into the rods or by pumping. The openhole method is feasible only within formations
that are fairly cohesive; otherwise, the formation
may flow upwards into the rods when they are
withdrawn, preventing samples from being collected. With single-rod systems, open-hole samChapter 8 Groundwater Sampling

pling can be conducted only at one depth within a


borehole because the borehole cannot be flushed
out between sampling intervals, which could
cause cross-contamination. Dual-tube systems, on
the other hand, can be used to conduct multilevel
sampling.
8.7.3. DPT Monitoring Well Installation
A variety of DPT methods are available for installing temporary or permanent monitoring
wells. The two main installation methods used
are exposed-screen and protected-screen wells.
These methods are discussed in detail in ASTM
D6724 and D6725, and are summarized here. As
with conventional well installations, hydraulic
connections should not be created between otherwise isolated water-bearing strata. In addition,
precautions should be taken to minimize turbidity
during the installation of filter packs and the
development and sampling of DPT wells.
8.7.3.1. Exposed-screen Well Installation
Methods
With exposed-screen well installation methods,
the well casing and screen are driven to the target
depth using a single string of rods. Because the
screen is exposed to formation materials while it
is advanced, proper well development is important to remove soil from screen slots. This method is not recommended for installing well
screens within or beneath contaminated zones
because drag-down of contaminants with the
screen may cross-contaminate sampling zones
and can prevent the acquisition of samples representative of the target zone. Exposed-screen well
installation methods should be used only in upgradient areas that are known to be uncontaminated. Also, some states prohibit the practice of
allowing the formation to collapse around a well
screen during the construction of a monitoring
well. Therefore, state regulations should be
consulted before selecting exposed-screen techniques.
8.7.3.2. Protected-screen Well Installation
Methods
When installing a protected-screen well, the well
casing and screen are either advanced within or
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lowered into a protective outer drive rod that has


already been driven to the target depth. Once the
well casing and screen are in place, the drive rod
is removed. Alternatively, the casing, screen, and
a retractable shield may be driven simultaneously
to the target depth. Once in place, the screen is
exposed and the entire unit remains in the ground.
If there is sufficient clearance between the inside
of the drive rod and the outside of the well casing
and screen, a filter pack and annular seal may be
installed by tremie (an apparatus for depositing
and consolidating concrete under water) from the
surface as the drive casing is removed from the
hole. Several filter packing and annular sealing
approaches are available, depending on the
equipment used for the installation. Regardless
of the method of installation, the filter pack
should be sized appropriately to retain most of the
formation materials.
The most common protected-screen method for
installing DPT wells is to advance an outer drive
casing equipped with an expendable drive tip to
the target depth. The well casing and screen are
then assembled, lowered inside the drive casing,
and anchored to the drive tip. The drive casing
seals off the formations through which it has been
advanced, protecting the well casing and screen
from clogging and from passing through potentially contaminated intervals. The position and
length of the screen should be selected to match
the thickness of the monitoring zone, which can
be determined by using additional information,
such as cone penetration testing (CPT) logs or
continuous soil boring logs.
8.8. Sample Handling and Collection
This section provides guidance on sample handling procedures, such as filtration, and specific
techniques for collection of samples that will be
analyzed for various classes of groundwater
pollutants, such as SVOCs. For detailed sampling procedures and preservation of samples,
refer to Appendix B of this handbook. It is important to remember that COC procedures should
be followed for all groundwater sampling events
and that all samples (except for metals) remain on
ice during both sample collection and shipment to
Chapter 8 Groundwater Sampling

the laboratory. Details regarding the use of COC


procedures are provided in Chapter 3.
8.8.1. Sampling for Metals
Certain regulations require metals analyses to be
performed on unfiltered groundwater samples.
The reason for these requirements is to obtain a
representative sample as it actually occurs in the
aquifer and to maintain consistency between
sample handling for inorganic and organic analyses. If a particular situation demands consideration of dissolved metals, both filtered and nonfiltered samples should be collected for analysis.
The regulatory document or approved SAP
should be consulted for monitoring requirements.
The differences obtained as a result of sample
handling (filtered versus non-filtered) are dependent on the type of association between the specific inorganic ion and the particulate matter.
Studies show that when an inorganic ion is not
closely associated with particulate matter (e.g.,
sodium), the differences between total and dissolved concentrations are small and random.
Ideally, the sample can be split into two portions,
one for filtration and the other for immediate
preservation and subsequent analysis for total
metals concentration. By analyzing the two
fractions separately, differences between dissolved and total metals can be compared.
The decision of whether to filter metals samples
should be based on the physical quality of the
samples, the objectives of the monitoring program, and the policy of the regulation or agency
controlling the sampling event. If filtering is
allowed and chosen, it is imperative that it be
performed in a manner that will preserve the
integrity of the sample and allow for consistent
reproduction of technique.
Filtration of groundwater samples for dissolved
metals analyses should be performed with a precleaned filtering apparatus. Sampling devices
should be cleaned using ultra-pure nitric acid
when low-level metals contaminants are being
measured. Filtration must be done immediately
upon sample collection, prior to preservation.
Samples transported to the lab for filtration and
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preservation should be documented, because


sample composition will change during transport.
The sample should be collected and filtered
through a 0.45-m pore diameter cellulose acetate
filter. If using a vacuum filter is impractical,
pressure filtration must be performed. Care
should be taken to follow the manufacturers
recommended procedure if vacuum filtration is
used. All filter apparatus should be laboratorycleaned and dedicated; however, disposable
filters are acceptable. For each sampling event, a
new disposable filter must be used to avoid crosscontamination of samples.
Groundwater samples to be analyzed for both
total metals and dissolved metals are collected in
plastic bottles and preserved with nitric acid to
pH < 2. All appropriate data should be recorded
in the FLB/FN.
8.8.2. Sampling for VOCs
At each site, samples for analysis of VOCs are
collected first. Care should be taken to prevent
volatilization of the sample when placing
groundwater into the vial. Groundwater samples
collected for analysis of VOCs, either from passive diffusion bags, low-flow pumps, or bailers,
must be placed into 40-milliliter vials with a
septum.
A sacrificial 40-milliliter sample should be obtained to determine preservation requirements
before VOC samples are collected. Fill the vial
with sample water, then add 1:1 HCl, drop-bydrop, and test the pH until it is < 2. If the test
sample effervesces when the HCl is added, the
samples should not be acid preserved and should
be analyzed within 7 days of collection. Record
the amount of HCl added. Alternatively, prepreserved VOC vials may be obtained from the
analytical laboratory.
The procedure for collecting a VOC sample is
described below:
1. Remove the cap from a 40-mililiter septum
(Teflon-faced silicon rubber) vial. Avoid
contact with the inner surface.

Chapter 8 Groundwater Sampling

2. Add the established amount of HCl necessary


for sample preservation (if prepreserved vials
have not been supplied by the laboratory).
3. Fill the vial with sample water, taking care to
minimize aeration, and screw on the cap
tightly to achieve zero headspace. The Teflon-lined side of the cap must face the
aqueous sample.
4. Inspect the vial for air bubbles. If air bubbles
are present, discard the vial and restart with
step 1.
5. Label the vial, and place it in a resealable bag.
6. Record appropriate data in the FLB/FN.
8.8.3. Sampling for Extractable Organics
The procedure for collecting groundwater samples for analysis of SVOCs is described below.
1. Remove the Teflon-lined cap from a 1-liter
amber glass bottle. Avoid contact with the inner surface of the cap.
2. Fill the bottle with groundwater.
3. Replace the cap tightly, attach the sample
label, and place the sample bottle in a cooler
with enough bagged ice to cool the sample to
6C.
4. Repeat steps 1 through 3 for additional samples.
5. Record appropriate data in the FLB/FN.
8.8.4. Sampling for Cyanide
The procedure for collecting groundwater samples for analysis of total cyanide is described
below.
1. Place groundwater into a 1-liter wide-mouth
plastic bottle.
2. Determine if sulfide is present. Pour a small
aliquot of sample from the 1-liter wide-mouth
plastic bottle into a clean 100-mililiter beaker
and test for sulfide using a lead acetate test
strip. If sulfide is:
Present and visible solids are present, go
to step 3
Present and no visible solids are present,
go to step 5

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3.

4.

5.

6.

7.

8.

9.

Not detected, go to step 8.


If sulfide is present and visible solids are
present, filter the sample through a 0.45-m
cartridge filter within 15 minutes of collection.
The sample should be pumped through the filter using new Tygon tubing into a second
clean, 1-liter wide-mouth plastic bottle.
Place the spent 0.45-m cartridge filter in a
1-gallon resealable bag, label the bag with the
appropriate sample number and collection
time, and place the filter cartridge and bag into
the freezer. The frozen filter can be sent to the
laboratory for analysis of cyanide.
For the presence of sulfide, add 1 gram of
solid lead carbonate to the 1-liter wide-mouth
sample bottle, cap the bottle, and mix by inverting the bottle several times.
Check for the removal of sulfide. Pour a small
aliquot of lead carbonate-treated sample into a
clean 100-milliliter beaker and test for sulfide
again using the lead acetate test strip. If sulfide is present, add another gram of lead carbonate to the sample, cap the bottle, and mix
by inverting the bottle several times. Repeat
this step until sulfide is not detected by the
lead acetate test strip.
Filter the lead carbonate-preserved sample
through a new 0.45-m cartridge filter to remove residual chemical addition and lead sulfide formed during the precipitation reaction.
Collect the filtrate in a clean 1-liter plastic
wide mouth bottle. Discard the 0.45-m cartridge filter.
Determine if total chlorine is present. Pour a
small aliquot of sample from the 1-liter widemouth plastic bottle (preserved, if sulfide was
present) into the appropriate vials of the chlorine test kit and analyze for total chlorine. If
total chlorine is present in the sample, add 0.1
gram of sodium borohydride (NaBH4), cap the
bottle, and mix by inverting the bottle several
times. If chlorine is not detected, go to step
10.
Check for the removal of chlorine. Pour a
second small aliquot of NaBH4-treated sample
into the appropriate vials of the chlorine test

Chapter 8 Groundwater Sampling

kit and analyze for total chlorine. If chlorine is


present, add another 0.1 gram of NaBH4. Repeat this step until chlorine is no longer detected. Generally, 0.1 gram/liter NaBH4 will
reduce 50 mg/liter of chlorine.
10. Adjust the pH of the sample to > 12 using
sodium hydroxide (NaOH), and place the
sample on ice to lower the temperature to
6C prior to shipping to the laboratory. When
the sample has cooled, pack and ship using
normal procedures. Record all preservation
procedures in the FLB/FN.
8.8.5.

Sampling for Conventional


Parameters and Nutrients
Conventional pollutants typically include BOD,
O&G/TPH, TOC, COD, TDS, TSS, and chloride.
Nutrients include ammonia, nitrate, and total
phosphorous. Bottle and preservation requirements will differ based on each particular analyte.
The procedure for collecting groundwater samples for analysis of conventional pollutants and
nutrients is described below:
1. Remove caps from sample bottles. Avoid
contact with the inner surface.
2. Fill bottles to about 90 percent full. Add
appropriate preservative to the samples per
Appendix B of this handbook or the SAP.
3. Replace and tighten caps, attach labels, seal in
resealable bags, and place sample bottles in a
cooler with enough bagged ice to cool the
samples to 6C.
4. Record all appropriate data in the FLB/FN.
8.8.6. Sampling for Radioactive Elements
Groundwater samples typically are analyzed for
the following radioactive constituents: gross
alpha, gross beta, tritium, strontium-90, combined
radium-226/228, and uranium. Other radioactive
elements, such as plutonium, cesium-137, or
americium-241, also may be included in groundwater sampling programs, depending on the
historical uses at the site. The types of sample
bottles and the required volume of the groundwater sample will vary depending on the radioactive
element. The SAP must contain information on
sample bottles, sample preservation, and sample
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holding times for specific radioactive elements


that will be analyzed. When preparing the SAP,
refer to the Multi-Agency Radiological Laboratory Analytical Protocols (MARLAP) guidance on
field sampling of radioactive analytes
(http://www.epa.gov/radiation/docs/marlap/402b-04-001b-10-final.pdf).
Note: Shipment of radioactive samples to the laboratory
may require special handling procedures. Samples to be
shipped off site must be field-screened to determine the
levels of radiation present. The screening will allow for
proper packaging and shipping via International Air Transport Association (IATA) Dangerous Goods Regulations.
By IATA definition, a material with an activity level of
more than 2,000 pCi/g is considered radioactive. If
groundwater samples exceed this level, special IATA
packaging procedures are required for shipment by air.
Packaging procedures for radioactive samples must be
included in the SAP, and special training of field personnel
may be required for the handling and packaging of radioactive groundwater samples.

8.8.7.

Sampling for Light, Non-aqueous


Phase Liquids
Light, non-aqueous phase liquids (LNAPLs) are
generally considered to be low density, immiscible organics, including gasoline, petrochemicals,
and other chemicals with specific gravities of less
than water. They are usually present in aquifers
as a separate phase due to their low solubility in
water. These chemicals tend to float on the water
surface in a water table environment and commonly occupy the capillary fringe zone above the
water table. If LNAPLs are suspected to be
floating on the water table, all shallow wells
installed in the area under investigation must be
screened across the water table.

Note: Samples of the floating organic layer must be


collected before the well is purged.

In a confined aquifer, LNAPLs are found along


the upper surface of the permeable material and
also within the overlying confining layer. When
immiscible organics with a specific gravity less
than water are the contaminants of concern, or if
contaminants are suspected in more than one
stratified layer in the well column, sampling
procedures must be modified. It may be necessary to lower the sampling bailer to a particular
depth in the well or to utilize a double checkChapter 8 Groundwater Sampling

valve bailer. Sampling procedures for LNAPLs


differ substantially from those for other pollutants. If more than one distinct LNAPL layer is
present in a well, each layer should be sampled.
Samples should be analyzed for chemical composition (e.g., for VOCs and base-neutral extractables) and physical parameters (e.g., specific
gravity, water solubility, vapor pressure of the
liquid, and Henrys Law Constant).
Measurement of the thickness of the floating
layer can be accomplished by using a water indicator paste or gel with a weighted steel tape to
determine the depth to the top of the floating
layer and to the water surface. The difference
between these two readings is the thickness of the
floating layer. Measurement of the thickness of
the floating layer also may be accomplished by
using an interface probe or a clear Teflon bailer
(if the product thickness is less than the length of
the bailer). Electric water level sounders will not
work properly for these determinations.
After a monitoring well is initially constructed, it
should be developed and pumped to remove
stagnant water. Then the well should sit idle for
at least 2 weeks to allow the water level and
floating layer(s) to stabilize fully. Prior to purging the monitoring well, a sample of the floating
layer can be obtained using a bailer that fills from
the bottom.
The collection of a water sample from a well
containing free-floating product is challenging
and at times problematic. This is true even if the
LNAPL floating in the well has been removed
during the purging process (the LNAPL can still
coat the inside casing, or be entrained in the
screen and sand pack, and likely is emulsified
below the air/water interface). Care should be
taken to lower the bailer just through the floating
layer but not significantly down into the underlying groundwater. Care also should be taken in
proper planning when sampling water from such
wells and interpreting the resulting data (e.g., to
determine if the sample is representative of the
actual groundwater concentrations). Various
sampling methods may be used to provide greater
confidence in the results of the analysis. Stilling
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tubes may be used to help prevent the sampling


device from contacting residual LNAPL that can
impact the collected water sample. Discrete
interval samplers also may be used to ensure that
emulsified product does not enter the sampler
during emplacement below the water level in the
well. Samples should be analyzed to determine
the chemical composition and physical properties
of the LNAPL. After following typical evacuation procedures discussed previously in this
section, a sample of formation water may be
obtained from the well.

the well by setting the pump intake of the submersible or suction-lift pump several feet above
the DNAPL.

8.8.8.

This section provides a brief discussion on sampling industrial wells used to extract process
water and potable water. Site Managers should
always consult the state environmental agencies
drinking water division to determine specific
requirements.

Sampling for Dense, Non-aqueous


Phase Liquids (DNAPLs)
DNAPLs include chlorinated solvents and other
chemicals with specific gravities greater than
water. They are usually present in aquifers as a
separate phase due to their low solubility in water. DNAPLs tend to migrate downward through
both the unsaturated zone and the saturated zone
due to their high density. If the volume of the
DNAPL introduced into the subsurface is larger
than the retention capacity of the vadose and
saturated zones, a portion of the DNAPL will
spread out as a layer of free liquid on the bottom
of the aquifer or on lower permeability beds
within the aquifer.
Measurement of the thickness of DNAPLs must
be performed prior to purging the well. Measurement of the DNAPL can be accomplished by
using a water indicator paste or gel with a
weighted steel tape (if no LNAPL is present) to
determine the depth of the top of the DNAPL and
the bottom of the well. The difference between
these two measurements is the thickness of the
DNAPL. An interface probe also may be used to
measure DNAPL thickness in the well.
Note: Samples of the settled organic layer must be collected before the well is purged.

Prior to purging the monitoring well, a sample of


the DNAPL can be obtained using a dual checkvalve bailer or a bladder pump. If both LNAPLs
and DNAPLs are present, it may be necessary to
purge the well of one casing volume of water
prior to sampling the DNAPL. Efforts should be
made not to disturb the DNAPL in the bottom of
Chapter 8 Groundwater Sampling

Samples should be analyzed to determine the


chemical composition of the DNAPL and its
physical properties (e.g., specific gravity, water
solubility, equilibrium vapor pressure of the
liquid, and Henrys Law Constant). After the
well is purged, a sample of the groundwater may
be obtained for laboratory analysis.
8.9. Sampling Industrial Wells

When sampling industrial wells, it is desirable to


sample as close to the well source as possible.
Samples should be taken directly from the well
head whenever possible to eliminate treatment
interferences, possible changes in quality within
the lines, and mixing of water from other wells.
Large-capacity wells that are on-line during
monitoring can be sampled immediately. Wells
that are off-line must be purged and pumped to
waste prior to sampling. Fifteen minutes or more
of pumping is suggested. Access to municipal
well systems, well houses, and other related
structures will require the assistance of the site
manager or water department employee. Prior
notification is essential.
8.10. Aquifer Testing
At sites with contaminated groundwater, aquifer
testing may be performed to determine sitespecific aquifer properties that help define the
transport of groundwater and contaminants. If
groundwater remediation is appropriate, an aquifer pumping test may be performed. During a
pumping test, groundwater is removed from the
aquifer for a period of several hours or days.
Sampling of the extracted water is required to
determine its disposal requirements. Samples are
typically collected from the containment vessel
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using a bailer, or directly filling sample bottles


from a port on the container.
Long-term aquifer tests can be used to estimate
contaminant loading on treatment systems by
collecting samples from a sample tap in the pump
discharge pipe at various times over the duration
of the aquifer test. This provides a more realistic
estimate of treatment system loading than using
individual samples collected from monitoring
wells. Use of monitoring well samples alone can
result in an overestimation of contaminant loading (and overdesign of the treatment process) if
groundwater concentrations decrease over the
course of the pumping test.
8.11. Well Decommissioning or Abandonment
This section provides an overview of the requirements for well decommissioning and abandonment. It is important that Site Managers
check with state environmental agencies to determine specific requirements.
Unsealed or improperly sealed groundwater
monitoring wells, including DPT wells, may
threaten public health and safety and the quality
of groundwater resources. Proper well abandonment accomplishes the following:

Eliminates the physical hazard of the well (the


actual hole in the ground)
Eliminates a pathway for migration of
contamination
Prevents hydrologic changes in the aquifer
system, such as the changes in hydraulic head
and the mixing of water between aquifers.
The proper decommissioning method will depend
on both the reason for abandonment and the
condition and construction details of the boring or
well.
Typically, well abandonment is the responsibility
of the property owner and must be done according to state regulations. In the absence of more
stringent regulatory standards, the procedures
outlined below represent minimum guidelines for
proper abandonment of wells and borings. These
steps may be applicable, but not limited to, public
and domestic water supply wells, monitoring
Chapter 8 Groundwater Sampling

wells, borings, or drive points drilled to collect


subsurface information, test borings for groundwater exploration, and dry wells (drains or borings to the subsurface).
1. The well should be plugged to prevent the
entrance of surface water, circulation of water
between or among producing zones, or any
other process resulting in the contamination or
pollution of groundwater resources.
2. The well should be chlorinated prior to abandonment using a chlorine solution with a minimum concentration of 150 ppm.
3. The entire depth of the well should be checked
before it is sealed to identify any obstruction
that could interfere with sealing operations.
4. The well bore should be filled and sealed
completely with bentonite cement grout.
5. The grout material should be placed in a way
that prevents voids in the grout or dilution of
the grout.
6. The abandoned well or bore should not become a channel for the vertical movement of
water or other substance to potable groundwater resources.
7. Upon completion of well abandonment, the
top of the casing and grout material should not
be terminated more than 4 feet below the
ground surface of the final grade.
8.12. Sampling Equipment List
Section 3.8 of this handbook provides a generic
sampling equipment list applicable to most sampling events. The following list provides additional equipment applicable to groundwater sampling. In most cases, only a portion of the equipment listed below would be required for a given
sampling event.

Water level indicator


Steel line and chalk
Electric tape (e.g., interface probe, slope
indicator, M-scope)
Well evacuation equipment
- Suction lift pump/centrifugal pump
- Portable submersible pump
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- Peristaltic pump
- Air lift pump
- Bladder pump (gas squeeze pump)
- Packer pump
- Gas piston pump
- Gas displacement pump
- Inertial pump
Groundwater sampling equipment
- Passive diffusion bags for VOCs
- Bottom fill bailer (single or double check
valve)
- Peristaltic pump
- Bladder pump
- Packer pump
- Inertial pump
- Syringe sampler
Additional equipment
- VOCs detection devices, such as PID or
FID
- Appropriate hand tools
- Keys to locked wells
- Filtering devices
- Field measurement instrumentation
(e.g., temperature, specific conductance,
pH, DO, turbidity)
- Plastic sheeting
- Dedicated, pre-cleaned stainless steel
pitchers, or an equivalent dipping device
- Calibrated bucket for purged water
measurement
- Distilled or deionized water or ASTM Type
II water
- Laboratory-grade glassware, detergent, or
cleaning materials
- Empty drums for collection of purged water
- Stainless steel clamps.

Chapter 8 Groundwater Sampling

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Chapter 8 Groundwater Sampling

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Chapter 9. Drinking Water Sampling


9.1. Purpose
This chapter provides standard drinking water
sampling procedures that accurately represent the
condition of drinking water and comply with
federal guidelines.
9.2. Background
The SDWA was passed in 1974 to protect public
health by regulating the nations public drinking
water supply. The law was amended in 1986 and
1996 to expand its scope and increase the number
of regulated contaminants. The SDWA authorizes EPA to set national health-based standards to
minimize the concentration of harmful contaminants in drinking water and protect the population
from naturally occurring or manmade pollutants.
Currently, there are 96 drinking water contaminants regulated under the SDWA.
The SDWA applies to every public water system
(PWS) in the United States. There are more than
170,000 PWSs that provide piped water for human consumption in the United States. A PWS is
defined as having at least 15 connections or
regularly serving at least 25 customers for at least
60 days per year. PWSs are classified as either
community water systems (CWSs), which number about 60,000, or non-community water systems (NCWSs), which number about 110,000. A
CWS supplies water to the same population year
round while a NCWS is defined by the population
served (e.g., transient or non-transient). A transient non-community water system (TNCWS)
serves the public, but not the same individuals,
for more than 6 months, such as in campgrounds.
A non-transient non-community water system
(NTNCWS) serves the public and the same population for more than 6 months, but not yearround, such as in schools. The majority of the
population in the United States receives drinking
water from a CWS. Household wells are exempt
from regulation, but the recent promulgation of
the Ground Water Rule (GWR) incorporates all
PWSs that use groundwater as a source.
While a TNCWS is monitored for a few contaminants (e.g., bacteria, nitrate, and nitrite), CWS
Chapter 9 Drinking Water Sampling

and NTNCWS monitoring is more extensive.


The breadth of monitoring required by the SDWA
is dependent on the section of the drinking water
system identified (e.g., source water, treatment,
distribution system, or tap), the number of customers, and the source of the water. Source water
(i.e., groundwater, surface water, or groundwater
under the influence of surface water) and the
point-of-entry into a water treatment system have
modest monitoring require-ments that are usually
handled by annual sampling for inorganic chemicals, nitrate, nitrite, radionuclides, synthetic organic chemicals (SOCs), VOCs, and asbestos. As the
drinking water progresses through the distribution
system, the microbiological monitoring requirements increase, as does the analysis for residual
disinfectant and contaminants related to treatment
and conveyance (e.g., trihalomethanes (THMs),
lead, and copper). For a utility serving more than
10,000 customers, as many as 50 microbiological
samples per month can be required. Section
9.7.2.4 indicates the number of samples that would
be required for smaller PWSs. To learn the exact
monitoring requirements for a particular drinking
water system, refer to 40 CFR 141 or the EPA
Interactive Sampling Guide for Drinking Water
System Operators
(http://www.epa.gov/safewater/smallsys/samplingc
d.html), or consult state drinking water program
coordinators.
The National Primary Drinking Water Regulations (NPDWRs) specify health-based, enforceable maximum contaminant levels (MCLs) for
specific pollutants found in drinking water or
require treatments to remove contaminants to a
safe level. The MCL is the concentration of
pollutant that will have no known or expected
risk to human health if consumed in drinking
water. Utilities are required to test for each applicable pollutant and ensure that the MCLs are
being achieved. The SDWA, as amended and
codified in CFR 141.151, requires utilities to
provide an annual report to customers attesting to
the condition of the water with the associated
MCLs.
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National Secondary Drinking Water Regulations


(NSDWRs) specify non-enforceable levels of
contaminants in drinking water that are intended
to mitigate suspected but unproven health risk
consequences, and conservatively serve as a goal
that providers of drinking water should strive to
meet maximum contaminant level goals
(MCLGs). MCLGs can carry some public health
considerations but also carry aesthetic characteristics such as taste and odor. An action level
(AL) is the maximum concentration of a contaminant that would have no adverse health effect if
consumed in drinking water. An AL is healthbased and, like an MCL, prompts aggressive
action by the utility to reduce the concentration of
the pollutant to safe levels. Usually ALs are
related to the treatment techniques applied to
drinking water.
Because of the SDWA, EPA has introduced a
number of rules to address specific problems
related to drinking water safety. The titles of
most of the rules are self-explanatory and result
in some additional monitoring and reporting. The
drinking water safety rules developed by EPA are
as follows.

GWR. Focuses on increased protection from


microbes in ground water.
Total Coliform Rule (TCR). Tightens the
SDWAs requirements on the concentration of
bacteria in treated water because positive
coliform tests can indicate treatment problems.
Surface Water Treatment Rule (SWTR).
Addresses the control of Giardia and viruses.
Subsequent revisions include Cryptosporidium
disinfection or removal.
Lead and Copper Rule (LCR). Deals with
potentially toxic levels of metals derived from
plumbing materials in the distribution system
and ways to minimize their concentration.
Tests that exceed the AL for lead or copper can
trigger extensive home monitoring.
Arsenic Rule (AR). Reduces the MCL for
arsenic from 50 g/L to 10 g/L. Additional
treatment could be needed to meet the new
MCL.

Chapter 9 Drinking Water Sampling

Disinfectants and Disinfectant Byproducts


Rule (DDBPR), Stage 1 and Stage 2.
Regulates the halogenated chemicals produced
by the disinfection of drinking water. THMs,
haloacetic acids (HAA5), Bromate, and
Chlorite are common disinfection byproducts
(DBPs) regulated by the EPA.
Unregulated Contaminants Monitoring
Rule (UCMR). Preserves the public health of
citizens by identifying new or emerging
pollutants associated with source water,
drinking water treatment, distribution systems,
and consumption.
Interim Enhanced SWTR. Created in
February 1999 to improve the control of
microbial populations, particularly
Cryptosporidium, while balancing the risks
from the production of disinfection byproducts.
Long-Term Stage 1 SWTR. Became
effective in January 2002 and built on the
control of microbial populations, specifically
Cryptosporidium. It strengthened the filtration
requirements, implemented the Stage 1 DBP
Rule, and incorporated smaller water systems.
Long-Term Stage 2 Enhanced SWTR.
Became effective in 2006 as a further
extension of the Cryptosporidium and
microbial control requirements of the earlier
rules. All systems using surface water or water
directly under the influence of surface water
are included. The rule requires routine
sampling for Cryptosporidium. Treatment
depends on the levels of Cryptosporidium
reported.
All of the sampling and analytical requirements
associated with the recently promulgated rules are
included in the EPA Interactive Sampling Guide
for Drinking Water System Operators and on
EPAs website, http://www.epa.gov/safewater.
9.3. Scope
This chapter provides the following procedures
for sampling groundwater and surface water
supplies for monitoring drinking water quality:

Microbiological, inorganic, and organic


sampling
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Monitoring of metals at the tap


Monitoring of turbidity levels for surface water
supplies.
To meet the requirements of the SDWA and the
related contaminant regulations, as well as ensure
the quality of a drinking water supply, a comprehensive drinking water sampling program must
be developed. The drinking water sampling
program should include detailed information
about the water source, entry point, treatment
process, and distribution system. This information will help samplers determine which monitoring requirements apply to a particular drinking
water supply. Monitoring requirements for
source water sampling or point-of-entry sampling
can be modest when compared with monitoring
requirements for points further along in a distribution system, or for a system serving a large
population. The drinking water sampling program must consider the monitoring requirements
for each component of the water distribution
system to ensure that all applicable regulations
are met. A comprehensive drinking water sampling program should compare samples collected
from the source water, entry point after treatment,
and distribution system to determine the effect of
treatment and plumbing systems on drinking
water quality.
9.4. Project Planning
This section describes the steps in planning a
drinking water sampling program. Before each
drinking water sampling program can begin,
concise objectives must be developed regarding
the intent of the sampling program. The objectives provide the framework for developing a
sampling strategy and preparing the sampling and
analysis plan.
9.4.1.
Sampling Strategy
The sampling strategy will help the project manager determine the appropriate sampling locations, sample numbers, and sample frequency
based on the following:

Water source
Source vulnerability
Analyses to be performed
Chapter 9 Drinking Water Sampling

Regulatory requirements
DQOs
The population served
Anticipated or potential contaminants
System size.

9.4.2.
Site-Specific SAP
A site-specific SAP should be prepared and reviewed by appropriate regulatory personnel prior
to starting any sampling event to ensure the proper location, parameters, and number of samples
are taken to meet compliance requirements. The
specific monitoring and reporting requirements of
the SDWA are beyond the scope of this handbook.
The site-specific SAP is an instruction manual for
field personnel. It should be built around the
objectives and sampling strategy. The SAP must
consider a variety of factors including the water
source, condition and accessibility of sampling
locations, suspected contaminants, analytical
methods and detection limits, collection methods,
sample handling procedures, and safety. See
Chapter 2 for a detailed discussion of SAP development applicable to all sampling programs.
Note: Site-specific sampling requirements are unique, and
local, state, and federal regulatory authorities should be
consulted to ensure the drinking water sampling program is
adequately prepared.

The SAP cannot be implemented effectively if


field personnel do not understand its contents.
Field personnel should fully understand the SAP,
and additional training should be provided prior
to field activities, if necessary.
9.4.3.
Certification
Some states might have certification programs
that require drinking water samples collected for
SDWA compliance be collected by approved
individuals. Some states also have certification
training programs and require samplers to be
certified for collecting drinking water samples.
Local health and environmental departments
require that water samples be collected in accordance with federal, state, or local regulations. A
review of the sampling plan must ensure that the

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samples collected will meet the necessary local


and state requirements for sampling personnel.

during transportation of the VOC samples to the


laboratory.

Only laboratories that are certified by the local,


state, or federal program with jurisdiction are
allowed to perform compliance testing for microbiology, inorganic, organic, and radiochemistry
analytes. However, any person acceptable to the
state can perform analyses for turbidity, chlorine
residual, and pH if primacy has been granted.

9.4.5.2. Field Blanks


Field blanks are samples of reagent water that are
transferred from one vessel to another at the sampling site. Typically, the laboratory will fill sample bottles with ASTM Type I or II water, seal the
bottles, and ship them to the sampling site along
with the empty bottles. The field crew will transfer the reagent water to another set of clean sample
bottles in the field and transport or ship the field
blanks with the actual samples to the laboratory.
This blank is used to show that the sampling procedures and atmosphere at the sampling site have
not caused contamination. Additional reagent
water should be available in field to ensure no air
bubble in field blanks.

EPA- or state-certified laboratories should supply


the blanks, containers, and preservatives for
sampling. These must be free of the contaminants at the detection levels. These materials
should be traceable and documented as free of
contaminants to aid the data reviewer and to
avoid resampling due to avoidable contamination.
9.4.4.
Analytical Methods
When taking samples for regulatory compliance,
EPA-approved methods must be used. Approved
methods are listed in 40 CFR 141 and Appendix
B of this handbook.
9.4.5.
Quality Assurance
Use the following protocol to ensure integrity and
accuracy of the data collected during drinking
water sampling. The laboratory analysis must be
performed by a certified laboratory for the method required.
All samples must be accompanied by a complete
COC record. Field blanks, trip blanks, and field
duplicates can be collected as part of the QA plan
to enable data evaluation for accuracy and integrity of drinking water sampling. QA/QC varies
with the regulatory requirements and site location
for each sample.
Detailed information on QA/QC, including the
systematic planning process, development of
DQOs, and preparation of QAPPs, is available in
Chapter 2 of this handbook.
9.4.5.1. Trip Blanks
Trip blanks (or transport blanks) should be prepared by the laboratory and usually consist of two
laboratory-filled vials in each container used to
ship water VOC samples. The trip blank is analyzed to show that contamination does not occur
Chapter 9 Drinking Water Sampling

9.4.5.3. Field Duplicates


Field duplicates are collected from fieldhomogenized samples, stored in two separate
containers, and analyzed separately at the same
laboratory. For VOCs, field duplicates are two
separate samples that are collected as close as
possible to the same point in space and time,
stored in separate containers, and analyzed separately at the same laboratory. These duplicates
are useful in documenting the precision of the
sampling process.
9.5. Hazards and Safety Precautions
A site-specific HASP that addresses all anticipated
hazards should be prepared for each task. Specifically, the HASP should address the following
hazards that could be associated with drinking
water sampling:

Exposure to biological and chemical


contaminants during sample collection
Exposure to reagents used for sample
preservation
Physical and biological hazards associated
with sampling sites specifically when
sampling surface waters or wells.
Refer to Chapter 2 of this handbook for specific
hazard identification techniques and detailed
control methods.

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9.6. General Sampling Procedures


General sampling procedures for each common
type of drinking water sampling are described in
this section.
9.6.1.
General Tap Sampling
General tap sampling is appropriate for most
drinking water sampling parameters and is the
most common drinking water sampling method.
9.6.1.1. Appropriate Parameters
Tap sampling is an acceptable sampling method
for the following parameters:

Inorganic contaminants
Microbiological
Metals
SVOCs
DPBs
Radionuclides.
9.6.1.2. Sampling Procedures
The general procedure for collecting samples
from a tap includes the following steps:
1. Determine the appropriate sample location
and assemble all necessary materials. The
proper preservative should be added by the
laboratory or be available in the field for addition to the sample. A dechlorinating agent is
used when sampling chlorinated waters (such
as those found in the distribution system).
Handle the sterilized containers carefully to
avoid contamination.
2. Go to the sampling location(s) specified in the
SAP. Drinking water sampling locations are
usually located in the distribution system and
are accessible during the day. Examples include hospitals, city buildings, restaurants,
pump stations, and dedicated sampling stations. The tap should be clean and in good
condition (i.e., no leaks). To minimize contamination, avoid drinking fountains and faucets with swivel necks unless specific pointof-use concerns arise. If the sampling location does not have an accessible tap, then a
separate, clean, 1-liter plastic or glass (as appropriate) container should be used to dip and
Chapter 9 Drinking Water Sampling

fill the sample bottle(s). Point-of-use filters


and leaking taps or faucets that allow water to
flow outside of the tap should be avoided.
3. Before turning on the tap, remove any aerator,
strainer, or hose to prevent contamination;
however, you might not be able to remove the
aerator or find a non-swivel faucet. The
screen should be removed prior to sampling
for bacteria or volatile organics because the
screen tends to aerate the water, resulting in
the loss of some organics and nonrepresentative samples. The removal of the
screen should be documented. When sampling for bacteria, do not take a sample from a
swivel faucet, because the joint can harbor a
significant bacterial population.
4. Open the cold-water tap, and allow the system
to flush to clear the service line from the
building to the distribution main. Allow the
water temperature to stabilize for 2 3 minutes before collecting the sample.
5. Fill out the sample label using waterproof ink.
Be sure to clearly identify the exact sample
collection location and the date and time of
collection. If the sample collection point has
a specific coded identification, include it on
the label and the COC record along with the
samplers name.
6. Adjust the flow from the tap to about 500
milliliters (1 pint) per minute (approximately
-inch diameter stream).
7. Check for steady flow. Do not change the
water flow once sampling has started.
8. Remove the bottle cap or open the plastic bag.
Add preservative if required. Position the
bottle or bag under the water flow. Hold the
bottle in one hand and the cap in the other.
When filling a bottle, tip the bottle slightly so
that water flows down the side wall of the
container. Fill the bottle to the shoulder about
inch from the top of the bottle. For VOCs,
fill the bottle just to the point of overflowing.
If using a plastic bag sampling container, fill
it to the marked fill line. If the preservative is
acid, add it after the sample is collected.
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WARNING: Do not lay the cap down or put it in a pocket.
Do not contaminate the sterile bottle (or bag), touch the
inside of the cap with your fingers, or permit the faucet to
touch the inside of the bottle or bag. Do not rinse out the
bottle or bag before collecting the sample.

9. For chlorinated systems, check the chlorine


residual and record; see Section 9.7.1.
10. Place the cap on the bottle and screw it down
tightly. If using a plastic bag, pull the wire
tabs and whirl the bag three times for a tight
seal.
11. Turn the tap off. Replace the aerator, strainer,
or hose.
12. Check that the information on the label is
correct.
13. Complete the necessary forms with the appropriate information, including the PWS
identification number, exact sample collection
location, date and time, and type of sample
(e.g., raw, tap, entry point, distribution system). Specify the type of analysis to be run.
Complete a COC record.
9.6.2.
Service Line Sampling
Service line sampling is required if a limited lead
service line replacement program is being considered or when the service line material is unknown.
9.6.2.1. Appropriate Parameters
Service line sampling is an acceptable method for
sampling metals.
9.6.2.2. Sampling Procedures
The general procedure for collecting samples
from a service line is as follows:
1. Determine the appropriate service line sample
location and assemble all necessary materials.
The proper preservative should be added by
the laboratory or available in the field for addition to the sample. Handle the sterilized
containers carefully to avoid contamination.
2. Fill out the label for the sampling bottle in
waterproof ink. Be sure to clearly identify the
exact sample collection location and the date
and time of collection. If the sample collection point has a specific coded identification,
Chapter 9 Drinking Water Sampling

include it on the label and the COC record


along with the samplers name.
3. Using one of the following three procedures,
ensure that service line water is being sampled:
a) At the tap, flush an appropriate volume of
water from the building plumbing before
collecting the sample. This removes the
water contained in the pipes between the
sampling tap and the service lines. Use a
container, such as a pitcher or bucket, for
measuring the volume of water wasted.
Table 9-1 provides an abbreviated list of
the volume to be flushed.
b) For single-family homes, allow the water
to run until there is a significant change in
its temperature. The temperature change
indicates that water is flowing from the
service line(s) outside the home.
c) Locate or install a sampling tap directly
on the service line, and sample from this
tap.
Table 9-1. Approximate Volume, in Gallons, of
Flush Water for Various Sizes and Length of
Copper Pipe
Nominal
Pipe Size
(inches)

Length of Pipe (inches)


10
0.1
.23
.41

20
0.2
.16
.82

30
0.3
0.4
1.2

40
0.4
0.9
1.6

50
0.5
1.1
2.0

100
1.0
2.3
4.1

4. After step 3a, 3b, or 3c, immediately collect


the sample in a 1-liter plastic bottle or collapsible container while the water is still flowing. For 3c, turn on the service line tap, and
collect the water immediately. Remove the
bottle cap, or open the plastic bag. Add preservative if required. Position the bottle or
bag under the water flow. Hold the bottle in
one hand and the cap in the other. Fill the
bottle to the shoulder, about inch from the
top of the bottle. If using a plastic bag sampling container, fill it to the marked fill line.

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WARNING: Do not lay the cap down or put it in a pocket.
Do not contaminate the sterile bottle (or bag), touch the cap
with your fingers, or permit the faucet to touch the inside of
the bottle or bag. Do not rinse out the bottle or bag before
collecting the sample.

5. For chlorinated systems, check the chlorine


residual and record; see Section 9.7.1.
6. Place the cap on the bottle and screw it down
tightly. If using a plastic bag, pull the wire
tabs and whirl the bag three times for a tight
seal.
7. Turn the tap off.
8. Check that the information on the label is
correct.
9. Complete the necessary forms with the appropriate information, including the PWS
identification number, exact sample collection
location, date and time, and type of sample
(e.g., raw, tap, entry point, distribution system). Specify the type of analysis to be run.
Complete a COC record.
9.6.3.
First-Draw Sampling
First-draw samples are taken to show compliance
with ALs. The water in the plumbing must stand
motionless in the pipes for at least 6 hours. Taps
within a work site building can be secured with
tape noting the date, time, and person securing
the area. Post signs to warn potential users not to
turn on the water during the test period.
9.6.3.1. Appropriate Parameters
First-draw sampling is an acceptable method for
sampling metals, particularly copper and lead.
9.6.3.2. Sampling Procedures
The following is a detailed first-draw sampling
procedure.
1. All samples for compliance monitoring must
be first-draw samples, taken from a kitchen
cold water or bathroom cold water sink tap;
avoid drinking water fountains. The proper
preservative should be added by the laboratory or available in the field for addition to the
sample. Handle the sterilized containers carefully to avoid contamination.

Chapter 9 Drinking Water Sampling

2. Fill out the sample label to indicate the date


and time of sample collection, the location,
type of samples, and the samplers name. The
site should be sealed, or a certification by the
homeowner must be signed to indicate the
length of time the system was not used.
CAUTION: Any use of the taps during the 6-hour rest
time that the tap is to be secured will invalidate that tap for
sampling. Do not turn valves or otherwise mechanically
shut down the tap as this can release high amounts of lead
and copper into the waterline. Secure taps by taping and
posting notices.

3. Before turning the tap water on, remove the


cap from the container and position the container under the kitchen or bathroom sink faucet. Turn on the cold water and begin filling
the container. Do not put the cap of the container down on any surface. Hold the bottle
in one hand and the cap in the other.
WARNING: Do not lay the cap down or put it in a pocket.
Do not contaminate the sterile bottle, touch the cap with
your fingers, or permit the faucet to touch the inside of the
bottle. Do not rinse out the bottle before collecting the
sample.

4. Fill the bottle to the shoulder, about inch


from the top of the bottle.
5. Turn off the water tap. Place the cap on the
bottle and screw it down tightly.
6. Check that the information on the label is
correct.
7. Complete the necessary forms with the appropriate information, including the PWS identification number, exact sample collection location, date and time, and type of sample (e.g.,
raw, tap, entry point, distribution system).
Specify the type of analysis to be run. Complete a COC record.
9.6.4.

Source Water Sampling (Surface


Water)
Source surface water sampling is appropriate for
drinking water parameters because initial contamination will determine the level of treatment required to be in compliance with federal, state and
local statutes.

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9.6.4.1. Appropriate Parameters


Source water sampling of surface waters is an
acceptable sampling method for the following
parameters:

Microbiological
Metals
SVOCs
Inorganic contaminants
Radionuclides.
9.6.4.2. Sampling Procedures
Refer to Chapter 6, Surface Water Sampling, for
further guidance and sampling procedures.
9.6.5. Source Water Sampling From a Well
Source water sampling from wells is appropriate
for most drinking water sampling parameters, as
it will determine the level of treatment required to
bring the water into compliance with federal,
state, and local statutes.
9.6.5.1. Appropriate Parameters
Source water sampling of wells is an acceptable
method for the following parameters:

Microbiological
Metals
SVOCs
Inorganic contaminants
Radionuclides.
9.6.5.2. Sampling Procedures
The general procedure for collecting source water
samples from wells is as follows:
Obtain as much information as possible from the
well owner, including depth of the well, well
yield, formation in which the well is completed,
screen depth and length, well construction material, diameter of casing and when and by whom
the well was installed. This information should
be verified if possible by obtaining drilling logs,
etc. With this information, the correct sampling
approach, as well as the number of gallons to be
evacuated, can be determined so that the collected
sample represents the condition of the groundwater.

Chapter 9 Drinking Water Sampling

1. When collecting a sample from an operating


domestic well, it is essential to evacuate the
plumbing and water storage tank. Running the
water for a minimum of 15 minutes before collection is a good rule of thumb; however, a
longer evacuation period is desirable. Listen for
the pump or the electric circuit to the pump to
come on, indicating that the plumbing is being
evacuated.
2. Determine if any treatment units are installed
on the system. Treatment such as softening,
iron removal, turbidity removal, disinfection,
and pH adjustment can provide misleading
analytical results depending on the parameters
of interest. Carbon filters for the removal of
organics are also increasingly popular and can
alter sampling results. If a treatment system
is in use, a basement or outside faucet can bypass such treated water.
Note: Sampling from the cold water faucet is preferred to
avoid samples heated by the water heater.

3. A brief inspection of the system should be


performed to locate the well, pump, storage
tanks, and any treatment systems. Samples
should be taken as close to the pumping well
as possible and prior to any storage tanks or
treatment systems. If a sample must be taken
following a treatment unit, the type, size, and
purpose of the unit should be noted in the
FLB/FN.
4. Faucets, particularly kitchen faucets, usually
have a screen installed on the discharge. The
screen should be removed prior to sampling
for bacteria or volatile organics because the
screen tends to aerate the water, resulting in
the loss of some organics, resulting in a nonrepresentative sample. The removal of the
screen should be noted. When sampling for
bacteria, do not take a sample from a swivel
faucet because the joint can harbor a significant bacterial population.
Note: A homeowners plumbing system should not be
tampered with in any way, except for removal of the faucet
screen with permission from the homeowner.

For long-term monitoring projects utilizing domestic wells, a specific tap or faucet should be
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designated as the target sample access point for


accurate reproducibility of future samples.
9.7. Parameter-Specific Sampling Procedures
Sampling procedures for regulated and unregulated contaminants are presented in this section by
group for the most frequently collected parameters.
Sampling procedures for newly regulated contaminants and other parameters of concern can be
found in EPA approved methods
(http://water.epa.gov/scitech/drinkingwater/labcert
/methods_index.cfm)
The parameters and method-specific QC are
found in the approved drinking water methods.
This section provides common parameter-specific
sampling procedures that meet federal requirements. State and local requirements can be different or more stringent; therefore, the sampler
should always check state and local sampling
requirements before the start of sampling.
9.7.1. Field Data
pH, temperature, chlorine residual, and turbidity
measurements are conducted in the field at the
start of sample collection.
9.7.1.1. Applicable Regulations
The SDWA requires EPA to institute rules and
regulations to ensure that drinking water is safe to
consume. The SWTR and subsequent amendments, were promulgated to minimize pathogen
contamination in drinking water. These are
discussed in Section 9.2. Disinfection and filtration for surface water and groundwater under the
influence of surface water is required.
Chlorine residual must be checked to determine
preservation, holding time, and, in the case of
bacteria testing, data interpretation. Chlorine
residual is measured when collecting samples in
the drinking water program as free chlorine residual. Total chlorine residual is measured by
water supply systems during treatment design,
process control studies, or for distribution system
problem solving.
MCL or Sampling Values. The regulator should
specify the requirements for pH, temperature, and
chlorine residual values for compliance. The
turbidity after conventional or direct filtration
Chapter 9 Drinking Water Sampling

should be 0.3 nephelometric turbidity units


(NTU) in 95% of all monthly samples collected.
At no time should the turbidity exceed 1.0 NTU.
Slow sand and diatomaceous earth filtration
systems must achieve a filtered water turbidity
level of 1 NTU in 95% of the measurements
each month (limits can vary by state). At no time
can the filtered water turbidity exceed 5 NTU.
9.7.1.2. Number and Frequency of Drinking
Water Samples
The pH, temperature, chlorine residual, and turbidity samples should be representative of the
systems filtered water. These measurements
should be collected once per day and at the start
of each sample collection. Turbidity must be
monitored every 4 hours on combined filter effluents, although individual states can reduce this
requirement to once-per-day for slow sand or
alternative filtration devices. For individual
filters, turbidity must be monitored every 15
minutes.
9.7.1.3. Sampling Locations
The regulator should specify where the pH, temperature, and chlorine residual samples must be
taken for compliance. One turbidity sample
should be taken at each entry point into the distribution system.
9.7.1.4. Analytical Methods
The free chlorine residual method uses the reagent diethylphenylenediamine (DPD) in a colorimetric test to determine the amount of free chlorine available for disinfection. Total chlorine
indicates how much of the added chlorine reacted
with the indigenous components in the sample
and can be determined by adding small amounts
of potassium iodide to the DPD solution and
recording the difference. The reagent used must
be clearly identified as measuring either free
chlorine or total chlorine. The results reported
must also indicate free or total chlorine measurements.
Nephelometery is a standard test method for
turbidity. It is based on comparison of the intensity of light scattered by the contained static
water sample under defined conditions to the
intensity of light scattered by a reference standard
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in the sample container. The higher the intensity


of scattered light, the higher the turbidity of the
sample.
9.7.1.5. Sample Volume
Sample volume depends on the method used for
each parameter; refer to Chapter 13 for a discussion of pH, temperature, and chlorine residual
field measurements. The turbidity volume collected should be sufficient to:

Ensure a representative sample


Allow for replicate analysis (if required)
Minimize waste disposal
Comply with the analytical method used.
9.7.1.6. Bottle Type
Bottle type depends on the method used for each
parameter; refer to Appendix B for a discussion
of pH, temperature, and chlorine residual field
measurements. Samples for turbidity should be
collected in plastic or glass bottles, as specified
by the selected analytical method.
9.7.1.7. Sampling Procedures
The field testing procedures for pH, temperature,
and chlorine measurements are presented in
Chapter 13. Chlorine residual test kits, including
instructions, are available for drinking water
testing to measure free or total chlorine. An
example of a chlorine residual method can be
found in Chapter 13. Most kits use DPD powder,
tablets, or drops of liquid placed in a glass tube
containing the sample. A color change after
adding the reagent indicates that free chlorine is
present. In some kits, the color is measured
against a field comparator or portable spectrophotometer showing concentration in mg/L or ppm.
If a free residual chlorine level of 0.1 ppm is
detected, this test will show as a trace of pink
color. Trace colors are visible by looking down
the tube and against a white background, which
ensures no reflection from any red or pink surrounding surfaces. Interferences in the measurement of chlorine can cause variations to the color
or affect the color formation. Any unusual color
formations or colors must be noted for proper
data interpretation. Note in the FLB/FN the
results in mg/L, the date and time of the sampler,
Chapter 9 Drinking Water Sampling

the name of the sample, as well as any observations made during the sampling or analysis. If
chlorine is not detected in the test, write not
detected.
A one-time demonstration of technician proficiency should be on file in the training records.
The one-time demonstration should include a
standard curve, a low-level measurement standard, and an annual performance evaluation
sample for chlorine and pH.
For turbidity sampling, all bottles must be thoroughly cleaned and rinsed with turbidity free
water prior to sample collection. Turbidity samples are collected typically during general tap
sampling, source water sampling from surface
water, and source water sampling from wells.
Refer to Sections 9.6.1, 9.6.4, and 9.6.5, respectively, for general sample collection procedures.
9.7.1.8. Preservation Requirements
There are no preservation requirements associated
with sampling pH, temperature, or chlorine residual. Ensure that samples for turbidity are cooled
to 6C.
9.7.1.9. Holding Time
Samples for pH, temperature, and chlorine residual must be analyzed immediately, which generally means within 15 minutes of sample collection. Samples for turbidity should be analyzed as
soon as possible after collection. If storage is
required, samples maintained at 6C can be
held for up to 48 hours.
9.7.2. Microbiological
This section covers specific sampling requirements for the following microbiologicals:

Coliforms
Cryptosporidium
Giardia.
9.7.2.1. Coliforms
Coliforms are a group of closely related bacteria
that are generally harmless, but do contain some
species that are human pathogens. They are
natural and common inhabitants of the soil and
ambient waters, such as lakes and rivers. Coliforms can be inactivated by treatment or die off
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naturally in a manner similar to most bacterial


pathogens and many viral pathogens. Therefore,
if coliforms are found in the distribution system,
pathogens also could be present.
9.7.2.2. Applicable Regulations
The TCR introduced in Section 9.2 was established by the SDWA with sample requirements
primarily based on the presence or absence of
total coliform bacteria rather than on the number
of coliforms detected in the samples. The TCR
exists to protect public health by determining the
presence of disease-causing pathogens in drinking
water.
The TCR became effective December 31, 1990
and supersedes the old National Interim Primary
Drinking Water Regulations (NIPDWR) for
maximum microbiological contaminant levels
(effective June 24, 1977). The rule requires that
total coliform-positive samples be further tested
for fecal coliform or Escherichia coli (E. coli)
and that a set of repeat samples be collected for
each total coliform-positive sample. When coliforms are detected, additional routine samples
must be collected the following month.
9.7.2.3. MCL
For systems collecting fewer than 40 samples per
month, no more than one sample per month is
allowed to be positive for total coliform. For
systems collecting greater than 40 samples per
month, no more than 5% of all monthly samples
are allowed to be positive. If a system exceeds
the monthly MCL, the public must be notified
within 14 days per the requirements established in
the Public Notification Rule. If an acute MCL
violation occurs (i.e., when any fecal coliform is
detected on a repeat sample) the public must be
notified within 72 hours.

Table 9-2. Microbiological Monitoring


Frequency for Routine Sampling in PWSs
Population Served

Minimum Routine
Samples/Month*

25 1,000

1,001 2,500

2,501 3,300

* The regulator can specify a sampling frequency of less


than once per month for selected systems. A CWS serving
more than 3,300 must refer to the CFR. Contact your state
drinking water representative for details.

Compliance with the TCR is based on the presence or absence of total coliform bacteria. If all
routine samples test negative (absent) for the
presence of total coliforms, no additional testing
is required for that monitoring period, regardless
of whether sampling is routinely conducted
monthly, quarterly, or annually. However, the
rule requires that total coliform-positive samples
(presence) be further tested for fecal coliform or
E. coli and that a set of three repeat samples be
collected for each total coliform-positive sample
monthly, quarterly, and annually. Systems that
collect one routine sample or fewer per month
must collect a fourth repeat sample. If total
coliforms are detected in any routine or repeat
sample, the sampler must collect at least five
routine samples the next month. Table 9-3 provides an abbreviated list of the required frequency
for repeat sampling.

9.7.2.4. Number and Frequency of Samples


The number of samples that must be taken
monthly is based on the population served by the
water system. Table 9-2 provides an abbreviated
list of minimum monthly monitoring requirements. Many community systems routinely
sample more than the minimum to monitor the
systems status.

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Table 9-3. Monitoring and Repeat Sampling


Frequency After a Total Coliform-Positive
Routine Sample
# of Routine
Samples/Month

# of Repeat
Samples

# of Routine
Samples
Following
Month

1/month*

5/month

2/month

5/month

3/month

5/month

* Or fewer.

All repeat samples must be collected within 24


hours of notification of the total coliform-positive
result, unless the state waives this requirement.
Each set of repeat samples must include the following:
One sample at the same tap as the original
sample
One sample within five service connections
upstream
One sample within five service connections
downstream.
If a system has only one service connection, the
state can authorize the system to collect the required set of repeat samples over 4 days, rather
than within 24 hours, after being notified of a
total coliform-positive result. Per state discretion,
such systems can collect a larger volume repeat
sample (or samples) instead of the standard 100milliliter container (e.g., a single 400-milliliter
repeat sample or two 200-milliliter repeat samples in one or more sample containers of any size
as long as the total volume collected is at least
400 milliliters). If a system collects more than
one routine sample per month, the total volume
required would be 300 milliliters.

form test and must be listed as approved for


compliance monitoring. EPA Method 1604 is
commonly used for total coliforms.
9.7.2.7. Sample Volume
The sample volume depends on the analytical
method used. However, at a minimum, one 100milliliter sample must be collected per test.
9.7.2.8. Bottle Type
Sample containers for collecting coliform samples must be sterilized, hold at least 120 milliliters (4 ounces) of water, and contain sodium
thiosulfate if the sampled water is chlorinated.
Bottles can be plastic or glass. The laboratory
normally supplies the container. Glass-stoppered
bottles must be covered with aluminum foil or
char-resistant paper prior to sterilization. The
covering on the top ensures that the seal between
the stopper and the bottle is not contaminated,
thus minimizing the potential for contaminating
the sample when it is opened. Some labs furnish
a single-service, sterilized, polyethylene bag or
bottle containing a sodium thiosulfate tablet. The
laboratory should perform sterility checks (one
per lot) prior to releasing the containers for collecting samples. The laboratory normally provides instructions to go along with the sample
containers it has supplied. Refer to those when
provided.
9.7.2.9. Sampling Procedures
The laboratory that supplies the sampling containers might provide instructions for the type of
monitoring being performed. Be sure to refer to
those instructions when provided. Total coliform
samples are collected typically during general tap
sampling, source water sampling from surface
water, and source water sampling from wells.
Refer to Sections 9.6.1, 9.6.4, and 9.6.5, respectively, for general sample collection procedures.

9.7.2.5. Sample Locations


Samples for the TCR are collected from the
distribution system based on the number and
frequency requirements.

9.7.2.10. Preservation Requirements


Coliform samples must be refrigerated or cooled
to 10Cimmediately after sampling.

9.7.2.6. Analytical Methods


The method used for fecal coliform and E. coli
analysis depends on that used for the total coli-

9.7.2.11. Holding Time


The laboratory must receive and begin analyzing
coliform samples within 30 hours of collection.
If the laboratory is nearby, refrigerate the samples

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with ice packs and deliver them directly. Samples analyzed by an off-site laboratory should be
shipped on ice via overnight service on the day
they were collected.
9.7.2.12. Cryptosporidium and Giardia
Cryptosporidium is a genus of protozoan parasites potentially found in water and other media.
The recent taxonomy of the genus Cryptosporidium includes two species that use humans as
hosts: C. hominis and C. parvum.
Giardia is a genus of protozoan parasites potentially found in water and other media. The recent
taxonomy of the genus Giardia includes one
species that uses humans as hosts: G. lamblia
(also called G. intestinalis or G. duodenalis).
Applicable Regulations. Under the 1996 SDWA
Amendments, EPA must supplement the existing
1989 SWTR with additional pathogen control
requirements. Several additions to the rule have
resulted in the Long-Term 2 Enhanced SWTR,
which focuses on the control of Cryptosporidium
and microbial pathogens.
MCLG. The Interim Enhanced Surface Water
Treatment Rule (IESWTR) has an MCLG of zero
or a 99% removal for systems that filter.
Number and Frequency of Drinking Water
Samples. Monitoring of source water is required
to determine the level of treatment for Cryptosporidium. Monthly samples are required for the first
2 years, with the level of Cryptosporidium determining the level of any subsequent treatment.
Most systems will not require additional treatment. A 6-year follow-up sample is required to
ensure continued compliance. Small systems can
monitor for E. coli and will monitor for Cryptosporidium only if the E. coli concentrations exceed
a specified level.
Sampling Locations. Samples are collected
from source water for distribution systems.
Analytical Methods. EPA Method 1623 can be
used to measure both Cryptosporidium and Giardia. Prior to analysis, the water sample must be
filtered and the extraneous materials retained on
the filter. Qualitative analysis is performed by
scanning each slide well for objects that meet the
Chapter 9 Drinking Water Sampling

size, shape, and fluorescence characteristics of


Cryptosporidium and Giardia oocysts. Quantitative analysis is performed by counting the total
number of objects on the slide confirmed as
oocysts. Quality is assured through reproducible
calibration and testing of the filtration, immunomagnetic separation (IMS), staining, and microscopy systems.
Sample Volume. The sample volume depends
on the analytical method used. Generally, 10-liter
bulk samples are taken.
Bottle Type. Ten-liter collapsible containers
generally are used for collecting Cryptosporidium
and Giardia. These containers must be sterilized,
and are normally supplied by the laboratory. The
laboratory should perform sterility checks (one
per lot) prior to releasing the containers for collecting samples. The laboratory typically provides instructions to accompany the sample containers. Refer to those when provided.
Sampling Procedures. The laboratory that
supplies the sampling containers can provide
instructions for the type of monitoring being
performed. Be sure to refer to those instructions
when provided. Cryptosporidium and Giardia
samples are collected typically during general tap
sampling, source water sampling from surface
water, and source water sampling from wells.
Refer to Sections 9.6.1, 9.6.4, and 9.6.5, respectively, for general sample collection procedures.
Preservation Requirements. Ambient water
samples are dynamic environments and, depending on sample constituents and environmental
conditions, Cryptosporidium and Giardia oocysts
present in a sample can degrade, potentially
biasing analytical results. Samples should be
chilled to reduce biological activity between
collection and analysis.
If samples are collected early in the day, they
should be chilled by storing in a refrigerator
between 1C and 10C or on ice in a cooler. If
the sample is pre-iced before shipping, the ice
should be replaced with fresh ice immediately
before shipment. If samples are collected later in
the day, these samples can be chilled overnight in
a refrigerator between 1C and 10C. This proPage 9-13

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cedure should be considered for bulk water samples that will be shipped off site because it minimizes the potential for water samples collected
during the summer to melt the ice in which they
are packed and arrive at the laboratory at > 20C.
If samples are shipped after collection at > 20C
with no chilling, the sample will not maintain the
temperature necessary to retard microbiological
activity and will not present a representative
sample for analysis.
PWSs shipping samples to off-site laboratories
for analysis should include in the shipping container a means for monitoring the temperature of
the sample during shipping to verify that the
sample did not freeze or exceed 20C. PakSense
labels adhere to the samples and provide accurate
readings of the temperature environment experienced by the samples in shipment.
Holding Time. Sample preparation must be
initiated within 96 hours of sample collection (if
shipped to the laboratory as a bulk sample) or
filtration (if filtered in the field). The laboratory
must complete elution, concentration, and purification in one workday. It is critical that these
steps be completed in one workday to minimize
the time that any target organisms present in the
sample sit in eluate or concentrated matrix. This
process ends with the application of the purified
sample on the slide for drying.
9.7.3.
Metals
EPA has determined that metals are health concerns at certain levels of exposure. Young children and pregnant woman are especially at risk
from high levels in their blood. Some of the most
pronounced effects in children are interference
with growth, deficits in IQ, and altered physical
and mental development.
Applicable Regulations. The SDWA has established MCLs for various metals (see Table 9-4).
The LCR applies to lead and copper and addresses the effects of plumbing materials on the
distribution system as well as ways to minimize
their concentration.
Table 9-4. Metal MCL or AL
Chapter 9 Drinking Water Sampling

Metal
Antimony

MCL (mg/L)
0.006

Arsenic

0.010

Barium

Beryllium

0.004

Cadmium

0.005

Chromium

0.100

Copper

AL= 1.3

Lead

AL= 0.015

Mercury

0.002

Selenium

0.05

Sodium
Thallium

20
0.002

Prior to December 1992, the MCL for lead was


0.05 mg/L. Since then, instead of establishing a
new MCL, a treatment technique requirement is
triggered by exceeding an AL. The AL for lead is
0.015 mg/L, and the AL for copper is 1.3 mg/L
measured at the 90th percentile at the consumer
tap. This means that some samples can exceed
0.015 mg/L for lead and 1.3 mg/L for copper and
still not exceed the AL. Specific rules for calculating the 90th percentile can be found in 40 CFR
141.80.
Number and Frequency of Samples. All systems must be monitored annually for all regulated
metals except for lead and copper. Sodium samples must be collected annually for surface waters, and every 3 years for groundwater sources.
In areas where the sodium content is variable,
more frequent analyses might be required. All
systems must be monitored for lead and copper
for a minimum of two consecutive 6-month periods until one of the following occurs.

Lead or copper concentrations exceed the


MCLs or ALs. Then, additional samples from
the distribution system and point of entry must
be collected for water quality parameters and
corrosion control treatment studies performed
and reviewed by state personnel.
Lead and copper concentrations meet the
MCLs or ALs for two consecutive periods.
Then, the water supply can petition the
regulator to reduce the number of tap water
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sampling sites and reduce the frequency of


collection.
The number of lead and copper samples taken
during the 6-month sampling period is based on
the population and the results from previous
samples. After two 6-month sampling periods of
meeting the MCL or AL, a system can request
reduced monitoring (see Table 9-5). Monitoring
frequency also can be reduced after several years
of meeting the AL. Refer to 40 CFR 141 for
specific information.

emission spectra by optical spectrometry. Samples are nebulized, and the resulting aerosol is
transported to the plasma torch. Element-specific
emission spectra are produced by a radiofrequency inductively coupled plasma. The
spectra are dispersed by a grating spectrometer,
and the intensities of the line spectra are monitored at specific wavelengths by a photosensitive
device. Photocurrents from the photosensitive
device are processed and recorded by a computer
system.

Table 9-5. Number of Samples for Standard


and Reduced Monitoring for Lead and Copper

Mercury can be analyzed using the automated


cold vapor technique. The flameless atomic
absorption (AA) procedure is a physical method
based on the absorption of radiation at 253.7 nm
by mercury vapor. The mercury is reduced to the
elemental state and aerated from solution. The
mercury vapor passes through a cell positioned in
the light path of an atomic absorption spectrophotometer. Absorbance (peak height) is measured
as a function of mercury concentration and recorded in the usual manner.

System Size
(Population
Served)

Number of
Number of
Sites (Standard Sites (Reduced
Monitoring)
Monitoring)

3301 10,000

40

20

501 3,300

20

10

101

500

10

up to 100

Sampling Locations. State-approved sampling


locations should be selected if any have been
designated. If not, representative sampling locations should be selected. First-draw samples
should be collected at cold-water taps in homes
and buildings that are at high risk for lead and/or
copper contamination. In addition, samples must
be obtained from each entry point to the distribution system (EPTDS). For a surface water system, the plant effluent tap might be an appropriate
sampling location. For a well discharging directly into a distribution system (also known as an
EPTDS), a tap on the wells discharge piping
after any treatment would be appropriate.
Analytical Methods. The method used for metal
analysis must be listed as approved for compliance monitoring. Inductively coupled plasmaatomic emission spectrometry (ICP-AES, EPA
Method 200.8) is a common method used for
metal analysis. The analysis involves multielemental determinations by ICP-AES using
sequential or simultaneous instruments. The
instruments measure characteristic atomic-line
Chapter 9 Drinking Water Sampling

If additional analytical sensitivity is required for


mercury (ng/L), EPA Method 1631, Mercury in
Water by Oxidation, Purge and Trap and Cold
Vapor Atomic Fluorescence Spectrometry
(CVAFS) can be employed. A water sample is
chemically treated to produce volatile mercury
and separated from the solution by purging with
an inert gas. The mercury is collected on a gold
trap and subsequently desorbed into a fluorescence spectrometer where the intensity of its
fluorescence is measured and compared with the
intensity of the standards. At this level of detection, precluding the introduction of contamination
is critical; care must be taken to insure that
clean/ultra clean sampling, transportation and
analysis techniques are used. Guidance on these
techniques can be found in Guidance for Implementation and Use of EPA Method 1631 for the
Determination of Low-Level Mercury (EPA 821R-01-023) and EPA Method 1631.
Sample Volume. Sample volume is specified by
the method or the laboratory. One-liter samples
are usually taken.

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Bottle Type. Sampling containers for metals can


be made of plastic or glass and should be 1-liter
in volume. A 1-liter plastic bottle is most commonly used.
Sampling Procedure. There are two types of
metal sampling procedures.
1. Service line sampling; see Section 9.6.2.
2. First-draw sampling; see Section 9.6.3.
Preservation Requirements. If the analytical
requirements are for total metals, field preservation is recommended. Samples are preserved by
adding approximately 3 milliliters of concentrated
ultrapure nitric acid to the sample bottle. Be
extremely careful when adding the acid. Check
the sample pH with litmus paper. Indicate if the
sample pH is < 2. If the pH is not < 2, add acid in
1-milliliter increments until the pH is < 2.
Record the amount of acid used, the ultimate
sample pH, the date and time of preservation, the
person performing the preservation, and the
source of the acid used. Indicate on the label
whether the sample has been acidified. If the
analytical requirements are for other than total
metals, check with the method for specific preservation techniques and requirements.
WARNING: Concentrated acids and other chemical
preservatives represent a safety concern. Refer to the
HASP and Chapter 2 for related precautions and PPE.

Holding Time. Samples can be shipped to the


laboratory and preserved by the laboratory within
14 days after sample collection. Samples preserved at the laboratory are not to be analyzed
until 24 hours after preservation. Preserved
samples should be analyzed as soon as possible,
but are stable (except mercury) for up to 6
months.
9.7.4.
Nitrates/Nitrites.
Nitrate is a form of nitrogen combined with
oxygen. It can be converted in the body to nitrite.
High concentrations of nitrate can cause serious
illness in infants less than 6 months of age. Nitrate, one of the most widespread of contaminants, can get into water if a well is improperly
constructed or located where it is subject to
sources of contamination.

Chapter 9 Drinking Water Sampling

Applicable Regulations. NPDWRs establish


MCLs for nitrates and nitrites.
MCL. The MCL for nitrate is 10 mg/L, and the
MCL for nitrite is 1 mg/L.
Number and Frequency of Samples. One
sample should be collected from each entry point
or from points in the distribution system that
represent each source or treatment plant. The
frequency of sampling for initial nitrate monitoring is one sample per quarter for surface water
and one annual sample for groundwater. If sample results are greater than 50 percent of the
MCL, then quarterly monitoring should be performed until four reliable and consistent sample
results that are less than 50 percent of the MCL
are obtained. The state may allow a reduced
sampling frequency for surface water (annually),
provided that analytical results from four consecutive quarters are less than 50 percent of the
MCL. For groundwater, the state may return
sampling frequency to annually after four consecutive quarterly samples are less than 50 percent of the MCL.
Sampling Locations. Drinking water compliance samples for nitrates and nitrites are taken
at the entry point to the distribution system after
treatment. Surface water supplies can take samples from the distribution system at a point that is
representative of each source after treatment.
Analytical Methods. If an ion chromatograph
(IC) is available, nitrates can be analyzed by EPA
Method 300. In this method, a small volume of
sample is introduced into an IC. The anions of
interest are separated and measured using a system consisting of a guard column, separator
column, suppressor device, and conductivity
detector.
Sample Volume. Sample volume is specified by
the method or the laboratory. One-liter samples
are usually taken
Bottle Type. Both nitrate and nitrite samples
should be collected in 1-liter glass or plastic
bottles.
Sampling Procedures. Nitrate and nitrite samples typically are collected during general tap
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sampling, source water sampling from surface


water, and source water sampling from wells.
Refer to Sections 9.6.1, 9.6.4, and 9.6.5, respectively, for general sample collection procedures.
Preservation Requirement. Samples should be
preserved per method requirements. All samples
should be packed on ice to lower the temperature
to 6C.
Holding Time. Nitrate and nitrite samples
should be delivered by the sampler or shipped to
the laboratory by overnight courier. Results can
be reported as nitrate/nitrite, nitrate only, or
nitrite only. Samples of non-chlorinated water
must be analyzed within 14 days. Nitrate from
chlorinated supplies must be analyzed within 28
days. Samples for nitrite must be analyzed within
48 hours of sample collection. When nitrite and
nitrate need to be determined separately, the
holding time of 48 hours for nitrite must be met.
9.7.5.

Pesticides and Synthetic Organic


Chemicals
Organic compounds that volatilize at temperatures greater than 150C and do not decompose
are termed semivolatile organic compounds
(SVOCs). The synthetic organic chemicals regulated by the SDWA are SVOCs that fall into the
categories of polychlorinated biphenyls (PCBs),
pesticides, fungicides, and herbicides. These
compounds are commercially produced with
applications for agriculture and home use. If
incorporated into the water supply, they could
impart significant health risks and are consequently regulated under the SDWA.
Applicable Regulations. Since the establishment of the SDWA Amendments of 1986, EPA
has established MCLs for PCBs, 23 pesticides,
and six other synthetic organic chemicals.
MCLs. A list of drinking water MCLs can be
found on the EPAs website,
http://water.epa.gov/drink/contaminants/index.cf
m.
Number and Frequency of Samples. For systems serving about 50,000 customers and operating within the MCLs, one sample per year is
required. For systems operating above the MCLs,
Chapter 9 Drinking Water Sampling

quarterly samples are required. The number of


samples required and frequency of sampling
varies with system size. Consult 40 CFR 141 or
http://www.epa.gov/safewater for additional
details.
Sampling Locations. State-approved sampling
locations should be selected if any have been
designated. If none have been designated, representative sampling locations should be selected.
Samples are collected after treatment at the treatment plant, or at the entry point to the distribution
system, making sure each individual source of
water is represented in the sample.
Analytical Method(s). The EPA 500 series
methods are designed to identify and quantify
organic compounds in municipal drinking water.
These methods are cited under the SDWA.
Sample Volume. Sample volume will vary with
the parameter being tested. Generally two 1-liter
samples are collected.
Bottle Type. All methods require the sample to
be collected in glass bottles with Teflon-lined
lids. The size and number of containers will vary
depending on the number of parameters to be
monitored. In most cases, samples are collected
in two 1-liter amber-glass bottles and preserved.
Exceptions exist and the methods must be reviewed prior to sampling to ensure the proper
size, number, and types of containers are selected.
Sampling Procedures. Samples for pesticides
and synthetic organic chemicals are collected
typically during general tap sampling, source
water sampling from surface water, and source
water sampling from wells. Refer to Sections
9.6.1, 9.6.4, and 9.6.5, respectively, for general
sample collection procedures.
Preservation Requirement. The preservatives
used vary in concentration, addition, and type,
depending on the method, parameters to be measured, and the matrix (refer to 40 CFR 141). All
samples should be cooled to 6C during transportation and storage. Chlorinated and nonchlorinated water supplies are preserved using
different preservatives. Preservatives include
sodium thiosulfate to remove chlorine, HCl to
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stabilize the pH and reduce biological activity,


and other chemicals such as mercuric chloride.
The use of mercuric chloride requires that the
samples and waste material be treated as a hazardous waste for mercury.
9.7.6.
DBPs
Chlorine and other chemical disinfectants have
been widely used by PWSs as a principal barrier
to microbial contaminants in drinking water.
DBPs are formed when disinfectants interact with
organic and inorganic materials in source waters.
The levels of DBPs in finished water also are
dependent on the pH, temperature, concentration
of precursor materials, and age of the water in the
distribution system. Drinking water can vary
significantly from one point in a distribution
system to another. The regulated DBPs included
in this section are:
Bromate
Chlorite
HAA5
Total trihalomethanes (TTHMs).
Applicable Regulations. DBPs are regulated
through the Stage 1 and Stage 2 of the DDBPR.
The Stage 1 DDBPR applies to water systems
that add a chemical disinfectant. The Stage 2
DDBPR, finalized in January 2006, makes incremental changes to the Stage 1 rule for additional
protection of public health.
The Stage 2 DDBPR is designed to protect public
health by supplementing existing drinking water
regulations with risk-targeted monitoring and
compliance determinations for MCLs. Under the
Stage 2 DDBPR, a water system will conduct an
evaluation of its distribution system to identify
the locations with high DBP concentrations.
These locations will then be used as the sampling
sites for DDBPR compliance monitoring. Monitoring is required for populations of over 10,000.
MCL. The MCL for each disinfection byproduct
covered in this section can be found in Table 9-6.

Table 9-6. DBPs/MCLs


Disinfection Byproduct
Bromate

MCL (mg/L)
0.010

Chlorite

1.0

HAA5

0.060

TTHMs

0.080

Number and Frequency of Drinking Water


Samples. The number of samples, frequency,
and location of monitoring is dependent on source
water, distribution size, initial monitoring results,
and state requirements. In general, sampling is
required annually for small ground water systems
and small subpart H systems. Sampling is required once per quarter for all other systems.
Sampling Locations. Samples are collected
within the distribution system after treatment.
Analytical Methods. Ion chromatography by
EPA Method 300 is a common method used for
the analysis of the inorganic fraction of DBPs. A
small sample volume is introduced into an IC.
The anions of interest are separated and measured
using a system consisting of a guard column,
analytical column, suppressor device, and conductivity detector. The organic DBPs are extracted and analyzed using gas chromatography
(GC) or GC/MS techniques. EPA Methods 501
and 524 are commonly used for TTHMs, and
EPA Method 552 is commonly used for HAA5.
Sample Volume. Sample volume is specified by
the method or the laboratory. Two 40- or 60milliliter samples are usually taken
Bottle Type. The laboratory normally supplies
the containers, preservatives, and blank water for
DBP sampling. Recommended containers are
glass, 60- to 120-milliliter screw-cap vials with a
Teflon-faced silicone septum. The preservatives, containers, and blank water should be
traceable and controlled to ensure no detectable
DBPs are present.
Sampling Procedures. DPB samples are collected typically during general tap sampling,
source water sampling from surface water, and
source water sampling from wells. Refer to

Chapter 9 Drinking Water Sampling

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Sections 9.6.1, 9.6.4, and 9.6.5, respectively, for


general sample collection procedures. Collect all
samples in duplicate, and prepare two field blanks
for each sampling site. Collect samples as follows:
1. Hold the vial at an angle, and fill it as near to
the top as possible without overflowing. Be
careful not to rinse out the preservative. No
air bubbles should pass through the sample as
the bottle is filled.
WARNING: Do not lay the cap down or put it in a pocket.
Do not contaminate the sterile bottle (or bag), touch the cap
with your fingers, or permit the faucet to touch the inside of
the bottle or bag. Do not rinse out the bottle or bag before
collecting the sample.

2. When sampling from an open body of water,


fill a clean, empty (no preservative), 1-quart,
wide-mouth bottle with sample and carefully
fill two sample vials from the wide-mouth
bottle. Discard the water in the wide-mouth
bottle after filling the vials.
3. If a preservative is to be added, do not completely fill the vial until after the preservative
has been added. After the preservative is
added, carefully fill the bottle.
4. When filling the bottle, form a meniscus (the
curved upper surface of a liquid formed by
surface tension) or gently pour sample water
from the vial cap to top off the bottle and
form a meniscus.
5. Screw the cap on the bottle so that the shiny,
Teflon side of the septum is in contact with
the water. Do not touch the septum, and do
not over-tighten.
6. Invert the bottle, tap against your other hand,
and check for air bubbles. If any are present,
add additional water to reform the meniscus
and check again until no air bubbles are
present.
WARNING: Air bubbles larger than approximately
1 millimeter can invalidate the sample. Glass vials must be
filled completely and handled with care to prevent spillage.

Preservation Requirement. For collecting


chlorinated samples, a dechlorinating agent such
as 25 milligrams ascorbic acid should be preChapter 9 Drinking Water Sampling

added by the laboratory supplying the sample


containers. If gases are not to be determined,
sodium thiosulfate can be used as the dechlorinating agent. It should rapidly dissolve as the bottle
is filled. For samples that require HCl, add one
drop of HCl to each 20 milliliters of sample
volume. Add the water before the HCl to ensure
that the HCl and sodium thiosulfate do not react
to form sulfur dioxide, which can affect the laboratory results. Sample pH should be < 2 after
adjustment. Table 9-7 gives a summary of recommended preservatives for different VOCs.
WARNING: Concentrated acids and other chemical
preservatives represent a safety concern. Refer to the
HASP and Chapter 2 for related precautions and PPE.

Table 9-7. Recommended Preservatives for


VOCs

Constituents

Chlorinated

Nonchlorinated

Halocarbons &
Aromatics

HCl + reducing HCl


agent

THMs

Reducing agent None required


(HCl optional)

Holding Time. Pack the samples and blanks


with ice to lower the temperature to 6C. Ship
to the laboratory by overnight courier or deliver
directly. Refer to method holding time requirements.
9.7.7.
Radionuclides
The EPA sampling requirement for radionuclides
is intended to improve public health protection by
reducing exposure to, and the related cancer risk
posed by, radionuclides.
Applicable Regulations. Since December 2003,
the Radionuclide Rule has included the existing
MCLs for combined radium-226 and radium-228,
gross alpha particle radioactivity, and beta particle and photon activity. The rule also established a new MCL for uranium. It is important to
note that the Radionuclide Rule regulates CWSs
only.
MCL. The MCL for each regulated radionuclide
can be found in Table 9-8.

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Table 9-8. Radionuclide MCL


Radionuclide
Alpha particles

MCL
15 picocuries per liter
(pCi/L)

Beta particles and photon


emitters

4 millirems per year

Radium-226 and radium228

5 pCi/L

Uranium

30 g/L

Number and Frequency of Drinking Water


Samples. Samples for radionuclides are collected
once every 4 years unless more frequent sampling
is required by the state. Initial monitoring is
performed by collecting one sample per quarter
for 1 year. Repeat monitoring can be reduced to a
single grab sample, if approved by the state. If
gross alpha particle activity is found to be above
the MCL, additional monitoring for radium-226
and radium-228 might be required. If the water
source is near nuclear facilities, additional parameters (e.g., tritium, strontium-89, strontium-90,
iodine-131, and cesium-134) might need to be
monitored. These additional parameters will be
specified in the state or federal permit.
Sampling Locations. State-approved sampling
locations should be selected if any have been
designated. If not, representative sampling locations should be selected. For a surface water
system, the plant effluent tap might be an appropriate sampling location. For a well discharging
directly into a distribution system (also known as
an EPTDS), a tap on the wells discharge piping
after any treatment would be appropriate.
Analytical Methods. Alpha particles are measured by reducing the sample using evaporation or
a suitable chemical method to the minimum
weight of material having measurable alpha
activity. Alpha radioactivity is measured by an
instrument composed of a detecting device, amplifier, power supply, and scaler the most widely
used being proportional, and scintillation counters. Gross alpha can be measured using EPA
Method 900.
Beta radioactivity can be measured by one of
several types of instruments composed of a deChapter 9 Drinking Water Sampling

tecting device and combined amplifier, power


supply, and scaler the most widely used being
proportional or Geiger-Muller counters. Where a
wide range of counting rates is encountered (0.1
1,300 counts per second), the proportional-type
counter is preferable due to a shorter resolving
time and greater stability of the instrument. The
test sample is reduced to the minimum weight of
solid material having measurable beta activity by
precipitation, ion exchange resin, or evaporation
techniques. Beta particles entering the sensitive
region of the detector produce ionization of the
counting gas. The negative ion of the original ion
pair is accelerated towards the anode, producing
additional ionization of the counting gas and
developing a voltage pulse at the anode. By use
of a suitable electronic apparatus, the pulse is
amplified to a voltage sufficient for operation of
the counter scaler. The number of pulses per unit
of time is related to the disintegration rate of the
test sample. Gross beta radiation also can be
measured using EPA Method 900.
Radium-226 and radium-228 are measured by
using sequential precipitation and an internal
proportional counter or scintillation counter.
Radium-226 and radium-228 in water are concentrated and separated by coprecipitation with
sulfates of lead and barium and purified by ethylenediaminetetraacetic acid (EDTA) chelation.
After 36-hour ingrowth of actinium-228 from
radium-228, actinium-228 is carried on yttrium
oxalate, purified, and beta-counted. Radium-226
in supernatant is precipitated as sulfate, purified,
and alpha-counted (per 7500-Ra B), or is transferred to a radon bubbler and determined by an
emanation procedure (per 7500-Ra C; the preferred method).
Solvent extraction technology is a common method for isolating and concentrating uranium in
drinking water by counting via a high-resolution
alpha-liquid-scintillation spectrometer. To determine total uranium, as well as limited isotopic
uranium (238U and 234U) by activity in drinking
water, a 200-milliliter acidified water sample is
first spiked with 232U as an isotopic tracer, boiled
briefly to remove radon, and evaporated until less
than 50 milliliters remain. The solution is then
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made approximately 0.01 M in diethylenetriaminepentaacetic acid (DTPA), and the pH is adjusted to between 2.5 and 3.0. The sample is
transferred to a separatory funnel and equilibrated
with 1.50 milliliters of an extractive scintillator
containing a dialkyl phosphoric acid extracting
agent. Under these conditions, only uranium is
quantitatively transferred to the organic phase
while the extraction of undesired ions is masked
by the presence of DTPA. Following phase
separation, 1.00 milliliters of the organic phase is
sparged with dry argon gas to remove oxygen, a
chemical quench agent, and counted on a highresolution alpha-liquid-scintillation spectrometer
and multichannel analyzer (MCA). Radium-226
can be measured using EPA Method 903, and
radium-228 can be measured using EPA Method
904.
Sample Volume. Sample volumes will vary
depending on the analytical requirement. Generally, 1 gallon is collected per sample. Sample
volumes being collected must be confirmed with
the laboratory performing the analysis.
Bottle Type. Containers suitable for radionuclide
sampling are either a one pre-cleaned 1-gallon
Nalgene plastic bottle, or two pre-cleaned 2-liter
plastic bottles per sample.
Sampling Procedures. Radionuclide samples
typically are collected during general tap sampling source water, sampling from surface water,
and source water sampling from wells. Refer to
Sections 9.6.1, 9.6.4 and 9.6.5, respectively, for
general sample collection procedures.
Preservation Requirement. Preservation for
radionuclides is based on the method, parameter,
and state requirements. Cesium-134 is preserved
with HCl to pH < 2. Tritium and iodine-131 are
not chemically preserved. All other regulated
radionuclide parameters are preserved with nitric
acid to pH < 2. If preservation is not performed
in the field, the preservative can be added upon
arrival at the laboratory. The preservative must
be added within 3 days of collection, and analysis
must not begin until 16 hours after acidification.
Preservatives must be checked for the absence of
the radionuclides being monitored.
Chapter 9 Drinking Water Sampling

Holding Time. Samples must be delivered to the


analytical laboratory within 3 days for proper
testing.
9.8. Sampling Equipment List
Section 3.8 provides a generic sampling equipment list applicable to most sampling events. The
following list provides specific equipment applicable to drinking water sampling.

Chlorine
- Chlorine test kit or DPD test kit
Microbiological
- 120 milliliters plastic or glass
containers (sterilized)
- Sodium thiosulfate a preservative
- 10-liter collapsible containers
Metals
- First Draw
1-liter bottle, plastic or glass
Nitric acid a preservative
Warning signs to notify potential users
not to turn on taps during testing
period
- Service Line Samples
Pitcher or bucket
Sampling tap
1-liter bottle, plastic or glass
Nitric acid a preservative
Synthetic Organic Chemicals
- Sulfuric acid (for nitrate nonchlorinated water only)
- Sodium thiosulfate a dechlorinating
agent
- HCl a preservative
- Mercuric chloride a preservative
- 1-liter amber glass bottles with
Teflon-lined lids
Note: Samples will be considered a hazardous material
once mercuric chloride is added.

DBPs
- 40-milliliter amber vials with Teflonfaced silicone septa
- Ascobic acid a dechlorinating agent
- HCl a preservative if sampling for
halocarbons or aromatics
- 1-quart wide-mouth bottle
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Radionuclides
- HCl a preservative if sampling for
Cesium-134
- Nitric acid a preservative for all
other radionuclides except for tritium
and iodine-131
- 1-gallon or two 1-liter plastic or glass
bottles, volume dependent upon
sample.

Chapter 9 Drinking Water Sampling

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Chapter 10. Waste Sampling


10.1. Purpose
This chapter provides general procedural guidance to technical personnel who sample underground storage tanks (UST), drums, cylinders,
articles containing PCBs, investigation derived
waste (IDW), and other sources of solid or hazardous wastes that pose a potential threat to
human health and the environment. Waste sampling may be performed for site assessments or
for meeting regulatory requirements mandating
proper storage, handling, and disposal of materials in drums, cylinders, USTs, articles containing PCBs, oil spills, and other solid wastes.

Specific objectives of waste sampling, as addressed in this chapter, are as follows:

10.2. Scope

Provide relevant data for the protection of


personnel
Determine the presence of any USTs, drums,
cylinders, articles containing PCBs, or other
solid or hazardous wastes that require special
handling
Determine waste characteristics such as
toxicity and physical hazards from reference or
known sources
Determine alternative disposal criteria in
accordance with federal, state, and local
regulations
Determine special procedural requirements for
the handling and sampling of PCBcontaminated articles, containers, and
transformers
Evaluate the SPCC plan (along with proper
health and safety procedures) to ensure that
spill sampling requirements are satisfied
subsequent to an accidental release from the
site
Define practices and procedures for safe
handling of drums and cylinders containing
solid or hazardous materials or wastes
Promote the safe handling of known hazardous
materials.

The overall objectives of waste sampling are to


determine waste composition and meet regulatory
monitoring requirements. Waste sampling activities need to be conducted properly to protect the
health of those carrying out the sampling and
ensure the accuracy and reliability of the sampling results. Waste sampling oversight should
be maintained by following a previously prepared
SAP; see Chapter 2 for more information. The
sampling procedures, documentation, packaging,
handling, and transportation requirements contained in the SAP should be followed. Refer to
Chapter 3 for a complete discussion of sampling
preparation and sample collection requirements
applicable to all types of sampling programs.

The following sampling subjects are included


within the scope of this chapter:

Note: Personnel should follow special precautionary


measures with unlabeled drums, cylinders, USTs, articles
containing PCBs, and other wastes unless their contents are
characterized or known.

USTs
PCBs
Containers and drums
Oil spills
Waste characterization
Surface sampling
Sewage sludge.

WARNING: Sampling personnel should be specifically


trained, qualified, and certified to perform waste sampling
operations due to the potential for encountering extreme
safety hazards during these operations.
Chapter 10 Waste Sampling

10.2.1. USTs
UST sampling provides information used to
determine compliance with regulations applicable
to USTs that contain petroleum products and
stored chemical substances. If locating the USTs
is an issue, then an electromagnetic wave device,
electrical resistivity meter, or ground-penetrating
radar can be used to estimate the location of
buried tanks.
The following references contain guidance on
UST sampling:
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40 CFR 112. EPA Regulation on Oil


Pollution Prevention
40 CFR 280. EPA Technical Standards and
Corrective Action Requirements for Owners
and Operators of USTs.
These references cover the following situations:

When tank volume, including piping, is


10 percent or more beneath the ground surface
When a tank holds RCRA hazardous wastes,
or a mixture of such wastes and other
regulated substances.
These federal regulations also outline procedures
for EPA approval of a state program to operate in
place of federal UST requirements. State standards must be no less stringent and must provide
adequate enforcement of compliance with these
standards. The sampling of USTs should comply
with all applicable federal, state, and local regulations pertaining to the management of listed
USTs. Sampling event planners should identify
the regulatory requirements (including the compliance of each UST) for sampling, monitoring,
and removal, where necessary.
10.2.2. PCBs
PCB sampling provides information and guidance
for PCB handling in accordance with applicable
federal, state, and local regulations.
The following references provide information on
PCB sampling, access, and storage:

TSCA. PCB requirements, as implemented by


EPA regulations
40 CFR 761. EPA regulations on PCB
Manufacturing, Processing, Distribution in
Commerce, and Use of PCBs and PCB Items.
Some regulatory requirements from the previously listed references are as follows:

Areas contaminated with PCBs in regulated


amounts must be closed to the public
All PCB transformers must be registered with
the appropriate fire department and labeled per
EPA requirements
PCB storage areas and transport vehicles
should be marked with special labels per
applicable DOT regulations
Chapter 10 Waste Sampling

Non-leaking PCB articles and equipment, or


leaking PCB items placed in non-leaking
containers, may be put in temporary storage
areas for up to 30 days
The site-specific SPCC plan should include
PCB sampling and follow proper health and
safety procedures for sampling personnel
PCB transformers or PCB-contaminated
materials must be moved to a permanent
storage facility if they have been stored in a
temporary facility for more than 30 days
PCB waste is subject to a 1-year time limit for
storage and disposal. Conditional extensions
can increase this limit by an additional year
(40 CFR 761.65)
Post-cleanup sampling should be performed to
verify conformance with cleanup standards (40
CFR 761.125).
When performing field sampling for PCBs, proper health and safety protocol must be followed in
accordance with OSHA 29 CFR 1910.120. All
items containing PCBs, or unknown items potentially related to PCBs, should be considered
potentially contaminated with PCBs and handled
according to regulations unless sampling results
prove otherwise.
10.2.3. Containers and Drums
Container and drum sampling provides information and guidance applicable to the regulation of
container and drum handling in accordance with
federal, state, and local regulations. Container
and drum sampling poses unique obstacles to
sampling personnel, including drum staging,
identification, and opening. Containers include
compressed gas cylinders.
The condition and content of drums will determine the appropriate procedures for handling
drums prior to sampling. All drums should be
visually inspected to gain as much information as
possible about their content. In most compliance
cases, the materials contained in the drum are
known. Appropriate procedures for handling the
suspected materials should be followed. However, depending on site control of the materials
placed in drums, additional safety practices
should be considered.
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Prior to drum sampling, a survey can be made to


classify the drums into preliminary hazard categories, such as the following:

Chemical incompatibility
Leaking or deteriorated
Bulging
Explosive or shock sensitive
Laboratory waste.
As a precautionary measure, all unknown drums
should be handled and sampled with a minimum
of Level B protection (per 29 CFR 1910.120) to
characterize the content of the drums. The drum
survey should also address unstacked and unorganized drums.
WARNING: Opening drums presents a major health and
safety hazard. Accidents may include detonation, explosion, fire, vapor generation, and physical injuries. Proper
precautionary measures must be taken while performing
drum sampling.

The following references provide information on


drum/container sampling:

OSHA 29 CFR 1910 and 1926. General


Safety and Health Standards and Safety and
Health Regulations for Construction
40 CFR 265. National Standards for the
Management of Hazardous Waste
49 CFR 171178. Established regulations for
the Safe and Secure Transportation of
Hazardous Materials in Commerce.
10.2.4. Oil Spills
Oil spill sampling offshore and ashore includes
the methodology to collect samples following
accidental discharge of oil from the site. Ashore
oil spill sampling is typically oil sampling at the
beach but should not be limited to only surface
sampling of the oil. There are two portions of
ashore oil spills that are important to sample: 1)
the surface layer (0 15 centimeters), which
reflects the accumulation of the oil from an offshore spill following washout to the beach, and 2)
long-term deposition of the contaminated products several feet deep at the beach.
The following references provide information on
oil spill sampling:
Chapter 10 Waste Sampling

40 CFR 109. EPA Regulation on Criteria for


State, Local and Regional Oil Removal
Contingency Plans
40 CFR 110. EPA Regulation on Discharge of
Oil
40 CFR 300. EPA Regulation on National Oil
and Hazardous Substances Pollution
Contingency Plan under CERCLA.
Oil spill sampling includes sampling the spill
first. Because each spill and spill site is unique, it
is impossible to establish step-by-step guidelines
for oil spill sampling. Spill samples should be
collected as soon as possible, gathering the greatest volume of oil before it spreads out or disperses. This technique also minimizes the effects
of weathering alteration on the spilled oil. Offshore and ashore oil spill sampling should be in
concurrence with the SPCC plan and the sitespecific HASP. The HASP provides technical
guidance associated with collection of samples.
10.2.5. Solid and Hazardous Waste
Characterization
Waste sampling provides the identification of
waste present, characterizes the waste, and aids in
the determination of adverse effects to human
health and the environment. This information
ultimately supports the selection of disposal
options available in accordance with federal,
state, and local regulations. RCRA, an amendment to the SWDA to ensure that solid wastes are
managed in an environmentally sound manner,
provides the following two distinct, yet interrelated, programs:

Subtitle D. Promotes and encourages the


environmentally sound management of solid
waste
Subtitle C. Promotes and encourages the
environmentally sound management of
hazardous waste.
10.2.5.1. Characteristics of Hazardous Waste
Characteristic hazardous wastes exhibit any of the
following:

Ignitability
Corrosivity
Reactivity
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Toxicity.
10.2.5.2. Ignitability
Ignitable hazardous wastes include the following:

Liquids (other than aqueous solutions)


containing less than 24% alcohol by volume
with a flash point of less than 60C (140F)
Non-liquids capable, under standard
temperature and pressure, of causing fire
through friction, absorption of moisture, or
spontaneous chemical changes and, when
ignited, of burning to create a hazard
Ignitable compressed gases
Oxidizers.
10.2.5.3. Corrosivity
Corrosive hazardous wastes include the following:
Aqueous solutions having a pH of 2 or
12.5
Liquids that corrode carbon steel at a rate >
6.35 millimeters (0.250 inch) per year.
10.2.5.4. Reactivity
Reactive hazardous wastes have any of the following attributes:

Cause explosions, toxic fumes, gases, or


vapors when heated compressed, or mixed
with water
Are normally unstable and readily undergo
violent change without detonating
Are cyanide- or sulfide-bearing wastes
Are capable of detonation or explosive
reaction when subjected to a strong initiating
source or heated under confinement
Are readily capable of detonation or explosive
decomposition or reaction at standard
temperature and pressure
Are listed as forbidden Class A or Class B
explosives.
10.2.5.5. Toxicity
A solid waste exhibits the characteristic of toxicity when the extract from a representative sample
of the waste contains any of the contaminants
listed in Table 1 of 40 CFR 261.24 at the concen-

Chapter 10 Waste Sampling

tration equal to or greater than the respective


value given in that table.
10.2.5.6. Listed Hazardous Wastes
Hazardous wastes are also listed in 40 CFR
261.31 34. These lists contain industry and
EPA hazardous waste numbers, descriptions, and
hazard codes (indicating type of hazard). Nonspecific source wastes such as degreasing solvents are assigned EPA hazardous waste designation numbers beginning with F. Wastes that
contain pure or commercial-grade unused chemical solvents are assigned EPA hazardous waste
designation numbers beginning with P or U;
commercial chemicals on these lists are regulated
as hazardous wastes when discarded. Note that
K-list wastes (hazardous wastes from specific
sources) involve in-process wastes and generally
are not applicable to this discussion.
10.2.5.7. Characterization by Sampling
Characterizing waste by sampling can be quite
expensive. It is preferable to identify wastes by
determining the origin of the waste. Once the
origin of the waste has been identified, knowledge of the process used to generate the wastes
(e.g., raw material consumption, products, and
by-products) can be used to narrow the list of
analytical methods required for characterizing
wastes. For containerized wastes, identifying
labels or reviewing paperwork associated with the
containers may also narrow the list of analytical
methods required. Associated paperwork may
include waste manifests, disposal logs, and
MSDSs. By reducing the number of analytical
tests required, the sampling costs, sample volumes, and resulting waste are reduced.
Field analytical techniques have made significant
improvements in rigor and credibility. Computerization and miniaturization are contributing to
technology improvements and innovations.
These improvements allow for more frequent use
of field testing to characterize wastes rather than
collecting samples and sending them to a laboratory for analysis. Field analytical methods may
be employed if sufficient documentation can be
provided to support the proper application of the
method. The selected field analysis method
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should demonstrate method quantitation limits


below the action level or levels of concern. Field
analysis allows for streamlining of the site investigation process.
10.2.6. Sewage Sludge
Sewage sludge sampling includes collecting and
analyzing representative samples of sewage
sludge prior to land application, surface disposal,
or firing in a sewage sludge incinerator. Sewage
sludge sampling also includes sampling of domestic sewage prior to disposal. Sampling data
allow for the characterization of sewage sludge to
determine disposal methods in accordance with
federal, state, and local regulations. The CWA
and RCRA are examples of two applicable federal regulations. The CWA regulates beneficial use
and disposal of sewage sludge, and RCRA regulates disposal of non-hazardous sludge in a municipal landfill and land disposal of hazardous
sludge.
Guidance for sewage sludge sampling is contained in the following references:

40 CFR 258. EPA Regulation on Criteria for


Municipal Solid Waste Landfills
40 CFR 268. EPA Regulation on Land
Disposal Restrictions
40 CFR 503. EPA Regulation on Standards
for the Use or Disposal of Sewage Sludge.
10.2.7. IDW
IDW is waste that is generated in the process of
investigating contaminated or potentially contaminated sites. IDW can include purge water,
cuttings from well installation, drilling mud, soil
from collection of samples, and contaminated
PPE. IDW should be sampled and disposed of in
accordance with the SAP, contractual requirements, and state and federal requirements. IDW
management has the potential for considerable
effort and expense, and should be considered
when planning an investigation. IDW will generally be sampled using the techniques described in
section 10.5 of this chapter.
For more information on managing IDW, consult
the EPAs Guide to Management of InvestigativeDerived Wastes
Chapter 10 Waste Sampling

(http://www.epa.gov/superfund/policy/remedy/pd
fs/93-45303fs-s.pdf).
10.3. Hazard and Safety Precautions
See Chapter 2 of this handbook for a discussion
of health and safety elements applicable to most
sampling programs. The following hazards,
discussed below, are specific to waste sampling:

Container hazards
USTs and other confined spaces
Explosive hazards.
10.3.1. Container Hazards
Reseal open bungs and drill openings as soon as
possible with new bungs or plugs to avoid vapor
release. If an open drum cannot be resealed,
place it into an overpack drum.
Bulging drums are extremely hazardous. Whenever possible, do not move drums that may be
under internal pressure, as evidenced by bulging
or swelling.
Laboratory packs (categorizing small containers
of chemicals, solvents, industrial supplies, etc. in
metal drums for disposal) can be an ignition
source for fires at hazardous waste sites, as they
sometimes contain shock-sensitive materials.
Treat such containers as explosive materials, and
use extreme care when opening these packs.
Prior to opening laboratory packs, make sure all
non-essential personnel are moved to a safe place.
Whenever possible, use a grappler unit constructed for explosives containment for initial
handling or sampling of such laboratory packs.
Sampling personnel should maintain continuous
communication with the Site Safety Officer until
operations are complete.
WARNING: If drums or cylinders show signs of swelling
or bulging, do not move or sample them until the pressure
can be relieved safely. If possible, relieve any excess
pressure prior to opening the drum by using a remotely
controlled device, such as a pneumatic impact wrench or
hydraulic penetration device. If pressure must be relieved
manually, place explosion-resistant plastic barriers between
the worker and the drums or cylinders.

10.3.2. USTs and Other Confined Spaces


For USTs and other confined spaces, the HASP
should be followed to ensure worker safety.
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WARNING: Personnel who enter a confined space should
be accompanied by an on-site standby unit at all times.

The following steps should be detailed in the


HASP prior to entry into a confined space:
1. Ventilate the area thoroughly prior to entry.
2. Disconnect connecting pipelines.
3. Take air samples to verify the absence of
flammable or other hazardous vapors and
demonstrate the presence of adequate oxygen
levels.
4. Provide entry and standby teams with proper
respiratory protection, protective clothing,
safety harnesses, and ropes.
5. Establish lifeline signals (e.g., tugging on a
rope) prior to entry so that field sampling personnel can communicate.
6. Maintain ladder(s) and other equipment in
accordance with OSHA regulations.
10.3.3. Explosive Hazards
Due to the inherent dangers in sampling explosives (as well as potential or suspected explosives), only those individuals who have been
trained and certified in the proper handling of
these materials should participate in sampling
activities. See OPNAVINST 8023.24B for qualifications and certification requirements. Special
considerations are required when sampling explosive wastes that may be susceptible to shock,
friction, electromagnetic radiation (EMR), electrostatic discharge, sparks, flames, elevated or
freezing temperatures, moisture, or sunlight.
Failure to handle explosives correctly could result
in damage to property, injury, or loss of life.
General safety considerations include wearing
PPE such as flameproof clothing, caps, safety
goggles or face shields, conductive shoes, and
respirators, if applicable. Only non-sparking
tools should be used. Electrical grounding may
be necessary in some cases. In addition, field
sampling personnel should collect the smallest
amount of sample necessary for the intended
testing and analysis.

WARNING: Only trained and certified explosives personnel should handle, sample, or test explosives or suspected
explosive materials.

10.4. Preparation
If the nature of the hazardous waste is unknown
(e.g., at an abandoned disposal site), sampling
personnel should take additional precautions to
protect themselves from direct contact with waste
materials. To characterize waste materials for
RCRA or to verify the contents in drums, cylinders, tanks, or transformers, it is important that
representative samples be collected and analyzed.
10.4.1. Preparation for UST Sampling
Before starting UST sampling, follow the hazard
and safety precautions specified in Section 10.3.
Prior to UST sampling, field personnel should
ensure there is no leakage of product from the
UST or related piping. If it is necessary to enter
into a tank or vault for sampling, strict procedures
for confined space entry should be followed by
qualified and experienced personnel.
10.4.2. Preparation for PCB Sampling
The toxic nature and degree of hazards posed by
PCBs require a high level of caution to be taken
during sampling. Appropriate protective gear and
clothing should be worn by sampling and support
personnel during sampling events. Proper gloves
should be used during sampling. Spill prevention
and control should be planned in advance if
transformer sampling is to be performed. Plastic
pads and sorbent materials should be available.
10.4.3. Preparation for Drum Sampling
Prior to initiation of a sampling event, all drums
should be inventoried. All available information
concerning each drum should be recorded in the
FLB/FN, including the following:

Chapter 10 Waste Sampling

Type of drum
Contents
Total capacity estimate
Markings
Labels
Color
Origin
Condition.
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Each drum should be marked with a unique identification number that corresponds to the sample
container for present and future reference. Enamel spray paint is suitable for this purpose.
Photographs of the numbered drum are useful for
documenting the condition of the drum and providing a permanent record.

10.4.3.1.2. Drum Deheader


A drum deheader can be used to open a drum
manually when the bung is not removable with a
bung wrench. Drum deheaders are constructed of
forged steel with an alloy steel blade designed to
cut the lid off (or partway off) with a scissor-like
cutting action.

The opening of closed drums prior to sampling


entails considerable risk if not performed with the
proper techniques, tools, and safety equipment.
Prior to sampling, all drums should be staged in
easy-access areas. Any standing water or other
materials should be removed from the top of the
container so that:

Drums are opened with a drum deheader by first


positioning the cutting edge just inside the top
chime and then tightening the adjustment screw
so that the header is held against the side of the
drum. The handle of the deheader is then moved
up and down while sliding the deheader along the
chime. If a drum has been damaged or badly
dented, it may not be possible to cut the entire top
of the drum. Because it is possible that the drum
is under pressure, field personnel should cut the
drum a small amount to release any pressure
before cutting the whole lid from the drum.
Proper health and safety procedures should be
followed when using a drum deheader.

1. The representative nature of the sample is not


compromised when the container is opened.
2. Water cannot enter drums containing waterreactive compounds.
Manual and remote drum sampling techniques are
discussed below.
WARNING: Before opening any drum, ensure that the
drum is in an area that has secondary containment.

10.4.3.1. Manual Drum Opening


Two tools, discussed below, are typically used to
open drums manually, bung wrenches and drum
deheaders.
10.4.3.1.1. Bung Wrench
The most common method for manually opening
drums is with a universal bung wrench. These
wrenches have fittings to remove nearly all commonly encountered bungs and are constructed
usually of cast iron, brass, or a bronze-beryllium
non-sparking alloy formulated to reduce the likelihood of sparks. Use of a non-sparking wrench is
highly recommended. However, use of a nonsparking wrench does not completely eliminate the
possibility of producing sparks.
The wrench fitting matching the bung is inserted
into the bung, and the tool is turned counterclockwise to remove the bung. Proper protection
and safety is necessary while opening drums.
WARNING: If drums or cylinders show signs of swelling
or bulging, do not move or sample them until the pressure
can be relieved safely.

Chapter 10 Waste Sampling

10.4.3.2. Remote Opening


Two devices, discussed below, are typically used
to open drums remotely, hydraulic devices and
pneumatic devices.
10.4.3.2.1. Hydraulic Devices
Remotely operated hydraulic devices use hydraulic pressure to pierce the wall of the drum. These
devices consist of a manually operated pump that
pressurizes oil through a length of hydraulic line.
The metal-pointed piercing device is attached to
the end of this line and pushed into the drum by
hydraulic pressure.
The piercing device attaches to the drum so that a
sampling hole is made in either the side of the
head or the lid. Some hollow or tube-like piercers are designed to be left in place as a permanent
tap or sampling port. Piercers are designed to
establish a tight seal upon penetrating the container.
10.4.3.2.2. Pneumatic Devices
Pneumatic devices use compressed air to remove
drum bungs remotely. A pneumatic bung remover consists of a compressed air supply that is
controlled by a heavy-duty, two-stage regulator.
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A high-pressure air line delivers compressed air


to a pneumatic drill, which turns the selected
bung removal fitting. An adjustable bracketing
system positions and aligns the pneumatic drill
over the bung. The bracketing system must be
attached to the drum before the drill can be operated.
10.4.4. Preparation for Cylinder Sampling
Compressed gas cylinder sampling and identification of unknown products pose great environmental and personal risks and should be performed only by persons with appropriate training
and experience. A local safety authority should
be contacted prior to sampling. A compressed
gas supplier may also be contacted for input.
Prior to initiation of a sampling event, all cylinders should be inventoried. The following information concerning each cylinder should be recorded in the FLB/FN:

Type of cylinder
Contents
Total capacity estimate
Markings
Labels
Color
Origin
Condition.
Each cylinder should be marked with a unique
identification number that corresponds to the
sample container for present and future reference.
Photographs of the numbered cylinders are useful
for documenting the condition of the cylinder and
providing a permanent record.
10.4.5. Preparation for Storage Tank,
Vacuum Truck, Process Vessel, and
Similar Large Container Sampling
Prior to initiation of a sampling event, all containers should be inventoried. The following
information concerning each container should be
recorded in the FLB/FN:

Type of container
Total capacity estimate
Actual capacity (if container is open)
Chapter 10 Waste Sampling

Markings
Labels
Color
Origin
Condition
Existence and condition of ladders and
catwalks.
Each container should be marked with a unique
identification number that corresponds to the
sample container for present and future reference.
Enamel spray paint is suitable for this purpose.
Photographs of the numbered vessels are useful
for documenting the condition of the containers
and providing a permanent record.
The procedure for opening a large containment
vessel will vary with different containers. Ideally, large tanks and pressure/vacuum containers
should be vented and opened for sampling by the
tank operator familiar with tank access processes.
Most large tanks and vacuum trucks have valves
near the bottom of the tank and hatches near the
top. It is preferable to collect samples from the
top of a tank for several reasons. First, the integrity of valves near the bottom of the tank cannot
be assured; the valve may be immobile, break, or
become jammed in the open position, resulting in
an uncontrolled release of the tank contents.
Second, the contents of a large vessel may become stratified, and collecting a sample from the
bottom will not permit the sampling of each
strata. The preferred method is to access the tank
from the top to obtain a cross-sectional sample of
its contents.
While opening and sampling larger containment
vessels, precautions should be taken to ensure
personal health and safety. Accessing storage
tanks requires a great deal of manual dexterity.
Such sampling usually requires climbing to the
top of the tank through a narrow vertical or spiral
stairway while wearing protective gear and carrying sampling equipment. At least two persons
should perform the sampling: one to open the
hatch and collect the samples and the other to
stand back (usually at the head of the stairway)
and observe, ready to assist or call for help.
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Prior to opening the hatch, sampling personnel


should check the tank for a pressure gauge.
Large tanks and pressure/vacuum containers
should be opened for sampling by the tank operator familiar with tank access procedures. However, if necessary, the release valve should be
opened slowly to bring the tank to atmospheric
pressure. If no release valve exists, field personnel should slowly loosen hatch cover bolts to
relieve the pressure in the tank. Personnel should
stop immediately if the pressure is too great or if
a release occurs. Hatch cover bolts should not be
removed until the tank is at atmospheric pressure.
If the tank pressure is too great or venting releases gases or vapors, field personnel should discontinue venting immediately. Sampling may need
to be postponed until the proper equipment is
available to control the release. Any atmospheric
releases should be measured with portable field
instrumentation and recorded in the FLB/FN.
10.5. Sample Collection Procedures
10.5.1. Large Tanks
Prior to sample collection, ensure that tanks are
stabilized, proper safety precautions are taken,
and backup personnel are in place. If the contents
of the tank are stratified, each stratum should be
sampled discretely. At a minimum, top, middle,
and bottom samples should be collected. If the
container has separate compartments, each should
be sampled separately at varying depths. Upon
retrieval of the sample, field personnel should
immediately transfer the sample into the sample
container.
Depending on the objective of the sampling event
(e.g., characterization for disposal), samples may
be composited in the laboratory on a weight/
weight or volume/volume basis prior to analysis.
Knowledge of the tank-filling process will guide
the decision of whether or not to composite. Hot
spots and separation of materials in compartments
may reduce disposal costs if only a portion of the
tank is contaminated. Compositing samples may
result in low reported laboratory concentrations
that are not representative of overall concentration. A well-designed sampling plan will ensure

Chapter 10 Waste Sampling

sampling accuracy and provide the data necessary


for decision making.
10.5.2. Secondary Containment Sampling
Secondary containment helps prevent serious
environmental problems by containing storage
container releases. While the storage container
itself is vital to minimize the potential for leaks,
secondary containment is another important
safeguard. The sampling of two types of secondary containment devices, barriers and doublewalled tanks, is discussed below.
10.5.2.1. Barriers
Barriers or dikes are used to contain releases from
storage containers and process units. The storage
containers are typically placed on an impermeable barrier such as a continuous concrete slab,
lined concrete slab, or geosynthetic clay liner.
For sampling inside this type of secondary containment, use one of the surficial sampling techniques discussed below.
10.5.2.2. Double-Walled Tanks and Interstitial
Spaces
Double-walled tanks are another common type of
secondary containment. In general, doublewalled tanks do not require barriers or dykes. For
USTs storing petroleum products, regulations
require monitoring of interstitial spaces to determine when primary containment has failed. For
USTs, liquids generally are not allowed to accumulate if systems are properly monitored. The
interstitial spaces of above-ground, double-walled
storage tanks often are not monitored; however,
tank integrity is checked regularly. Over time,
small leaks may allow liquids to accumulate in
interstitial spaces. For sampling interstitial spaces, use one of the containerized liquid sampling
techniques discussed in Section 10.5.5. Depending on container construction, there may be limited access to interstitial spaces for sampling.
10.5.3. Surficial Sampling
Surficial sampling is used to assess the existence
or extent of contamination on surfaces rather than
in a soil, liquid, or air matrix. For example, the
interior of a building may be assessed by collecting wipe samples from process vessels and intePage 10-9

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riors of ventilation ducts. Though wipe, chip,


sweep, and rinsate sampling have similar purposes, they are intended to assess different types of
surface areas.

1. Premeasure the area to allow for easier calculation of final results. If premeasuring is not
feasible, measurements may be taken after the
area is wiped.

This recommended protocol outlines procedures


and equipment for the collection of representative
wipe, chip, sweep, and rinsate samples.

2. Wearing a new pair of surgical gloves, remove the gauze pad from its sterile wrapping
container and soak the gauze pad with the appropriate solvent.

10.5.3.1. Wipe Samples


Wipe sampling is intended to monitor surficial
contamination of non-volatile species of analytes
(e.g., PCBs, metals, tetrachlorodibenzo-p-dioxin
(TCDD), and tetrachlorodibenzofuran (TCDF) on
non-porous surfaces, such as metal or glass.
Sampling points should be chosen carefully and
based on site history, manufacturing processes,
personnel practices, obvious contamination,
migration pathways, and available surface area.
Suggested sampling points include process vessels, ventilation ducts and fans, exposed beams,
and window panes. The sampling area should be
large enough to provide a sufficient amount of
sample for analysis (smaller sample amounts
result in higher detection limits).
To collect a wipe sample, the following equipment is needed:

Ruler or measuring tape to measure out the


area being wiped
3-inch by 3-inch gauze pad inside a precleaned container
Sample container
Appropriate collection solvent
Surgical gloves, changed prior to handling
clean gauze, the sample container, or solvent.
The use of filter paper for wipe sampling is not
recommended because it tends to rip and crumble
on rough surfaces. If filter paper is used, it
should be 4-inch-diameter heavy gauge paper,
such as Whatman #4 filter paper.
Once the sample location is determined, sample
collection can begin. For each sample, a new pair
of surgical gloves should be worn to avoid cross
contamination of the collected samples. The
following procedure should be used for taking
wipe samples:

Chapter 10 Waste Sampling

3. Applying moderate pressure, wipe the entire


sample area once in the horizontal direction
and once in the vertical direction.
4. Wipe the entire sample area so that all sample
material is picked up.
5. Place the gauze pad in the sample container.
A field blank should be collected for every lot of
wipe material or solvent used. In some cases,
blanks may be collected every 10 wipes to provide additional data for interpretation. Field
blanks help identify potential contaminants from
the pad, solvent, sample container, or ambient air.
To perform a wipe blank, start by wearing new
gloves, then wet a gauze pad with the solvent or
water (for each collection parameter) and place
the pad directly into the sample container.
In some cases, the laboratory should be told to
rinse each sample container with an appropriate
extraction or digestion solvent (depending on the
analysis being performed) when transferring a
sample to the extraction glassware. This procedure will ensure that the entire sample is removed
from the container.
10.5.3.2. Chip Samples
Chip sampling is intended to monitor surficial
contamination of non-volatile species of analytes
(e.g., metals, PCBs, TCDD, and TCDF) on porous surfaces (e.g., cement, brick, and wood).
Sampling points should be chosen carefully based
on site history, manufacturing processes, personnel practices, obvious contamination, and available surface area. Suggested sampling points
include floors near process vessels and storage
tanks and loading dock areas. The sampling area
should be large enough to provide a sufficient
amount of sample for analysis (smaller sample
amounts result in higher detection limits). To
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facilitate the calculations once the analytical data


is received, the sample area should be measured.

obvious contamination, migration pathways, and


available surface area.

To collect a chip sample, the following equipment is needed:

Suggested sampling points include areas in


ventilation systems where dust can collect, floor
surfaces near process vessels and storage tanks
(e.g., linoleum floors where a solvent cannot be
used or too much residue exists for a wipe sample to be easily collected), and street gutters
where contaminated sediments may have migrated and accumulated. The sample area
should be large enough to provide a sufficient
amount of sample for analysis.

Ruler or measuring tape to measure the area


to be sampled
Surgical gloves, changed prior to collecting
each sample
Decontaminated chisel of borosilicate
construction and a manual or electric hammer
Natural bristle brush and a dustpan lined with
aluminum foil or one that is dedicated,
decontaminated, and constructed of a preapproved material that will not interfere with
the contaminants of concern
Sample container.
Once the sample location has been determined
and marked off, sample collection can begin.
The following procedure should be used for
collecting chip samples:
1. Measure the sample area (for calculation of
final results).
2. Break up the sample surface using a decontaminated chisel and hammer. Avoid scattering pieces beyond the sampling boundary.
Any pieces that fall outside the sampling
area should not be used. Chip depth should
be less than inch (preferably inch).
3. Record chip depth in the FLB/FN.
4. Collect the chipped pieces using a dedicated,
decontaminated dustpan and natural bristle
brush, and transfer the sample directly into
the sample container.
10.5.3.3. Sweep Samples
Sweep sampling is intended to monitor surficial
contamination of non-volatile species of analytes
(e.g., metals, PCBs, TCDD, and TCDF) in residue found on porous (e.g., asphalt) or nonporous (e.g., metal) surfaces. Sweep sampling
collects dust and residue samples that may help
determine and delineate contaminants. Sampling points should be based on site history,
manufacturing processes, personnel practices,

Chapter 10 Waste Sampling

To collect a sweep sample, the following equipment is needed:

Natural bristle brush


Decontaminated stainless steel spatula and/or
a dustpan lined with aluminum foil or one that
is dedicated, decontaminated, and constructed
of a pre-approved material that will not
interfere with the contaminants of concern
Surgical gloves, changed prior to collecting
each sample
Sample container.
Once the sample location is determined, sample
collection can begin. Wearing a new pair of
surgical gloves, sweep all residues in the sample
area onto the dustpan or directly into the sample
container. A dedicated, decontaminated spatula
may be used to aid in transferring the sample
into the sample container.
10.5.3.4. Rinsate Samples
Rinsate sampling is intended to determine if
surfaces contain hazardous waste residue after
being cleaned. This type of surficial sampling is
associated normally with drum storage pads,
floors of buildings, and the interior walls of
waste tanks.
Rinsate samples are performed by collecting
water from the last rinse step during the cleaning
of a tank or surface area. The water is analyzed
for known chemical contaminants and compared
against a blank sample of the same type of water.

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10.5.4. Transformers
The many peculiarities associated with transformers warrant that they be considered separately
from drums and tanks. Because transformers
often are located in secured, out-of-the-way
locations, access may be a problem. A poweroperated scissor lift or cherry picker may be
needed to access pole-mounted transformers. In
other cases, the transformer may be in an underground cell.
Special precautions should be taken due to the
toxic nature and hazards posed by PCBs, which
may be present in a transformer. Appropriate
protection should be worn by sampling and
support personnel. To aid in spill prevention
and control, make sure to use plastic sheeting
and absorbent pads
WARNING: Prior to sampling, transformers must be
certified as off line and de-energized by an electrician
or other authorized person. Internal pressure should be
relieved before opening the transformer.

Once power to the transformer is cut and spill


control measures are in place (plastic sheeting
on ground or floor surface of lift), the cover of
the transformer can be removed with hand tools.
A sample of the dielectric fluid can be obtained
with a disposable glass composite liquid waste
sampler (COLIWASA); see Section 10.5.5.2.
The following procedure should be used to
obtain a representative sample from the transformer:
1. Lower the COLIWASA at a rate that allows
fluid levels on both the inside and the outside
of the sampler to equalize.
2. Close the COLIWASA when it reaches the
bottom of the transformer and, as the
COLIWASA is retrieved, wipe it with a disposable absorbent pad.
3. Transfer the sample directly into the sample
container. If a disposable sampling device is
used, and if the transformer is out of service,
it may be possible to leave the used sampler
in the sampled material; however, this should
be done only after consultation with responsible authorities. Otherwise, the sampler
Chapter 10 Waste Sampling

should be drummed along with protective


clothing, sheeting, and absorbent pads, and
disposed of at a predetermined approved location.
Note: Never use the transformer drain valve for sample
collection for the following reasons:
1.

The integrity of these valves cannot be assured; the


valve may be rusty, may break, or may become
jammed in the open position, resulting in the uncontrolled release of transformer contents.

2.

Transformer contents may be stratified. Because


PCBs are heavier than other insulating oils, the resulting stratification may prevent collection of representative samples. Samples obtained from the valve
near the bottom of the transformer might indicate
higher PCB concentrations than the true concentration
of the total dielectric fluid.

10.5.5. Containerized Liquids


Liquids stored in a container are some of the
most difficult to sample. Several factors determine which method to use for sampling containerized liquids, including container location,
size and location of the container opening, and
type of equipment available for sampling. The
health and safety of sampling personnel also
plays a key role in determining sampling methodology.
No matter what type of sampler is chosen, it
should allow for the collection of all phases
present in the container. Containers rarely hold
a homogeneous mixture of material.
Sampling devices and their procedures for use
with containerized liquids are presented below.
Other appropriate sampling devices include the
Bacon bomb sampler, Kemmerer sampler, and
weighted bottle sampler (see Chapter 6).
Sampling containerized liquids presents unique
obstacles to sampling personnel. Procedures for
container staging, identification, and opening
should be well planned. Health and safety precautions associated with sampling containerized
materials are generally more stringent. QA/QC
guidelines for waste samples, as opposed to
environmental samples, are unique; therefore,
each site should be considered individually. If
high levels of contaminants are expected, trip
and field blanks may be needed. However, if
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residual or low-level waste or chemicals are


expected in the sampled material, trip and field
blanks may not be needed. If VOCs analyses are
being conducted, trip and field blanks are required.
All containers should be inventoried prior to the
initiation of the sampling event. The following
information concerning each container should be
recorded in the FLB/FN:

Type of container
Estimated total capacity of individual
container
Actual container capacity
Markings, labels, color, origin, condition, etc.
Photographs may also be taken to provide a
permanent record.
Depending on the container location and position, it may be necessary to upright and/or relocate containers prior to sampling. Containers
that can be moved should be positioned so that
the opening, or bung, is upright, if the integrity
of the container will allow. Containers should
not be stacked.
WARNING: Drums containing liquid waste can be under
pressure or vacuum. A bulging drum should not be
moved or sampled until the pressure can be relieved
safely.

The sampling of tanks, containers, and drums


presents unique problems. Waste containers
have various access ports including small access
ports, manways, or hatches on the larger vessels
or taps and bungs on smaller drums. The physical size, shape, construction material, and access
location of each vessel will limit the types of
equipment and methods that can be used for
sample collection.
When liquids are contained in sealed vessels, gas
vapor pressures build up, sludge settles out, and
density layering develops. The potential for
explosive reactions or the release of noxious
gases when containers are opened requires considerable safeguards. The vessels should be
opened with extreme caution. Certain situations
may warrant preliminary sampling of headspace
gasses. At a minimum, a preliminary check with
Chapter 10 Waste Sampling

an explosimeter or an organic vapor analyzer


will help determine levels of personnel protection and may aid in selecting a sampling method.
In most cases, it is impossible to observe the
contents of sealed or partially-sealed vessels.
Since some layering or stratification is likely in
any undisturbed solution, a sample should be
taken that represents the entire depth of the
vessel.
Agitation of vessel contents to disrupt the layers
and rehomogenize the sample is physically
difficult and almost always undesirable. In
vessels greater than 1 meter in depth, the preferred sampling method involves slowly, and in
known increments of length, lowering the suction line from a peristaltic pump. Discrete samples can be collected at various depths and combined or analyzed separately. If the specific
depth of the sample is important, a discrete
sampling device, such as the Kemmerer type,
may be required. In situations where the reactive nature of the contents is known, a small
submersible pump may be used.
When sampling a previously sealed vessel, a
check should be made for the presence of bottom
sludge by measuring the depth to the apparent
bottom and then comparing it to the known
interior vessel depth.
Liquid samples from containers such as 55gallon drums may be collected using lengths of
glass tubing known as drum thieves. These
tubes are normally 122 centimeters in length
with a 6- to 16-millimeter inside diameter.
Larger diameter tubes may be used for viscous
fluids if sampling with the small diameter tube is
not adequate. Sampling using the drum thief
requires a two-person sampling team (minimum)
and proper protective gear. Use of a drum thief
is simple, relatively inexpensive, quick, and does
not require equipment decontamination; however, this method does have serious drawbacks.
Most low-density fluids do not hold well in the
glass tubes. A significant amount of the potential sample flows out of the bottom of the tube as
it is raised from the drum, thereby reducing the
representativeness of collected material. Many
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variations to this technique have been reported,


including the incorporation of a small suction
device (e.g., a pipette bulb) to the top of the
tube, as well as the use of various tube sizes.
Some success has been reported with tubes that
have been heated at one end and then drawn to
form a smaller orifice. This technique allows for
the use of larger diameter tubing, which collects
a larger sample volume per attempt, while reducing material loss from the bottom of the tube.
The COLIWASA is a sampler designed for
representative sampling of multiphase wastes
from drums and other containers. The
COLIWASA is commercially available or can be
fabricated from a variety of materials, including
PVC, glass, or Teflon. A COLIWASA usually
consists of a 152-centimeter by 4-centimeter
(inside diameter) tube with a neoprene stopper at
one end, attached by a rod running the length of
the tube to a locking mechanism at the other end.
Manipulation of the locking mechanism opens
and closes the sampler by lowering and raising
the neoprene stopper. A recommended model of
the COLIWASA is shown in Figure 10-1. However, the design can be modified or adapted to
meet the needs of the sampling event.
Figure 10-1. COLIWASA Sampler

for those containing solvents. A glass


COLIWASA is suitable for wastes that are unsuitable for the plastic unit, except for strong
alkali and hydrofluoric acid solutions. Due to the
unknown nature of most containerized wastes,
samplers composed of glass or Teflon are preferred in lieu of samplers containing PVC.
To identify stratified drum content and sample
stratified samples, lower a glass COLIWASA into
a drum all the way to the bottom slowly to allow
the sample in the COLIWASA to equalize with
the material in the drum, and then visually examine the withdrawn sample for stratified layers
and depths. The stratified layers in the
CALIWASA may be individually transferred to
sample containers, or another COLIWASA may
be used to collect stratified samples at the specific
depths.
The major drawbacks associated with using a
COLIWASA involve potential decontamination
requirements and higher costs.
Specific procedures for using the drum thief and
COLIWASA are provided below.
10.5.5.1. Procedures for Drum Sampling Using
Glass Tubes (Drum Thieves)
The following method is recommended for using
glass tubes.
1. Record the drum identification number or
label for later confirmation, sampling, or disposal.
2. Open the drum.
3. Remove the cover from the sample container.
4. Lower the glass tubing until it almost touches
the bottom of the container. Keep at least 30
centimeters of tubing above the top of the
container.
5. Allow the sample in the tube to equalize with
the material in the drum.
6. Cap the top of the tube with a safety-gloved
thumb or a rubber stopper.

The COLIWASA is used primarily to sample


containerized liquids. The PVC COLIWASA can
sample most containerized liquid wastes except
Chapter 10 Waste Sampling

7. Carefully remove the capped tube from the


drum, and insert the uncapped end into the
sample container.
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8. Release the thumb or stopper covering the


tube, and fill the sample container to approximately 90% capacity or until no headspace
remains for volatiles.
9. Repeat steps 2 7 if more volume is needed
to fill the sample container.
10. Remove the tube from the sample container,
and replace the tube in the drum.
11. Cap the sample container tightly with a Teflon-lined cap, and attach the sample identification tag.
12. Replace the bung, or place plastic over the
drum.
13. Place the sample container in a resealable
plastic bag (one per bag). Place the bag in a
clean paint can for transport.
14. Mark the sample identification number on the
outside of each paint can, and complete the
COC record and the FLB/FN.
The following optional method is recommended
if a sample of the bottom sludge is desired:
1. Remove the covers from the container opening and the sample container.
2. Lower the glass tubing until it almost touches
the bottom of the container. Keep at least 30
centimeters of tubing above the top of the
container.
3. Allow the sample in the tube to equalize with
the material in the drum.
4. Gently push the tube toward the bottom of the
drum into the sludge layer. Do not force it.
5. Cap the top of the tube with a safety-gloved
thumb or rubber stopper.
6. Carefully remove the capped tube from the
drum, and insert the uncapped end into the
sample container.
7. Release the thumb or stopper covering the
tube, and allow the sample container to fill to
approximately 90% capacity or until no headspace remains for volatiles. If necessary, the
sludge plug in the bottom of the tube can be

Chapter 10 Waste Sampling

dislodged with the aid of a stainless steel laboratory spatula.


8. Repeat steps 2 7 if more volume is needed
to fill the sample container, and recap the
tube.
9. Proceed as in steps 10 13 above.
Note: If a reaction (e.g., violent agitation, smoke, and/or
light) is observed when the glass tube is inserted, field
sampling personnel should evacuate the area immediately.
If the glass tube becomes cloudy or smoky after insertion
into the drum, then hydrofluoric acid might be present.
Therefore, a comparable length of rigid plastic tubing
should be used to collect the sample. When a solid is
encountered in a drum (either in a layer or as bottom
sludge), the method described above for sampling bottom
sludge may be used to collect a core of the material. The
material may also be collected with a disposable scoop
attached to a wooden or plastic rod.

10.5.5.2. COLIWASA Use Procedures


The following procedures can be adapted for use
with other versions of COLIWASA samplers:
1. Select the COLIWASA material, assemble
the sampler, and ensure the sampler is clean.
2. Check to make sure the sampler is functioning
properly. If necessary, adjust the locking mechanism so the neoprene rubber stopper provides a tight closure.
3. Wear the necessary PPE, and observe required sampling precautions.
4. Open the sampler by placing the stopper rod
handle in the T-position and pushing the rod
down until the handle sits against the sampler's locking block.
5. Slowly lower the sampler into the liquid
waste at a rate that permits the levels of the
liquid inside and outside of the sampler tube
to equalize. If the liquid level in the sample
tube is lower than the liquid level outside the
sampler, the sampling rate is too fast and will
result in a non-representative sample.
6. When the sampler stopper hits the bottom of
the waste container, push the sampler tube
downward against the stopper to close the
sampler. Lock the sampler in the closed posi-

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tion by turning the T-handle upright and resting one end tightly on the locking block.
7. Slowly withdraw the sample from the waste
container with one hand while wiping the
sampler tube with a disposable cloth or rag
with the other hand.
8. Carefully discharge the sample into a suitable
sample container by slowly pulling the lower
end of the T-handle away from the locking
block with the lower end of the sampler positioned in the sample container.
9. Cap the sample container with a Teflonlined cap, label the container, and complete
the COC record and the FLB/FN.
10. Unscrew the T-handle of the sampler, and
disengage the locking block. Clean the sampler on site, or store the contaminated parts of
the sampler in a plastic storage tube for subsequent cleaning. Store used rags in plastic
bags for subsequent disposal.
10.5.6. Waste Pile Sampling
The protocol discussed below outlines general
procedures for collecting samples from waste
piles and other waste materials, equipment necessary for sampling, and adequate representation of
the material. This section also discusses factors to
consider when formulating a sampling plan. Due
to the many variables associated with waste
material sampling, exact procedures cannot be
outlined for every sampling situation. These
variables include the following: shape and size of
piles; size, compactness, and structure of the
waste material; and make-up. To determine the
correct sampling methodology, the chemical and
physical properties of a sample, the purpose of
the sampling event, analysis procedures, and the
intended use for the analyzed data should all be
considered when planning the sampling event.
10.5.6.1. Considerations for the Sampling Plan
The physical and chemical make-up of the waste
pile and the purpose for sampling should be
considered when planning the sampling event.
Considerations for creating a waste pile sampling
plan are presented below.

Chapter 10 Waste Sampling

10.5.6.2. Shape and Size


The shape and size of waste material and waste
piles can vary greatly. Piles may be cone-shaped,
long and rectangular, square, oval, or irregularly
shaped. State and federal regulations often require a specific number of samples per volume of
waste; therefore, size and shape may be used to
calculate volume and plan for the correct number
of samples. Shape also should be considered
when planning physical access to the sampling
point and selecting the type of equipment necessary to safely and successfully collect the sample
at that location.
10.5.6.3. Sampling Procedures
Waste pile samples can be collected at the surface
or at depth. These samples generally are collected using one of the following samplers: trowel
or scoop, waste pile sampler, sampling trier, soil
auger, grain sampler, split-spoon sampler, or soil
coring device. Surface samples can be collected
most efficiently with a trowel or a scoop. For
samples at depth, augers may be used. For a
sample core, waste pile samplers or grain samplers may be used.
For surface sampling, clear surface debris and use
a trowel or scoop to collect a sample at a depth of
0 6 inches. The depth of surface samples may
be determined by federal, state, or local regulations. Typically, the top 6-inch soils should not
be analyzed for VOCs due to evaporation and
loss. For surface core sampling, use a waste pile
sampler, trier, or similar sampling device. Transfer the sample directly into the sample container
with a decontaminated trowel or spatula (if necessary). A wide mouth bottle is preferred because it
requires less disturbance of the sample when it is
transferred into the sample container. If homogenization will be performed in the field, it should
be performed prior to transferring the material to
sample containers.
When sampling at depth, clear away the initial
top layer of material prior to taking samples, and
advance the hole to the desired sampling depth
with a decontaminated bucket auger or power
auger. Use a separate decontaminated sampler to
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minated spatula to transfer the sample into the


sample container.
Sampling devices most commonly used for small
waste piles include thieves, triers, and shovels.
Evacuation equipment, such as backhoes, can be
useful for sampling larger waste piles.
A thief consists of two slotted concentric tubes,
usually made of stainless steel or brass (see Figure 10-2). The outer tube has a conical pointed
tip that permits the sampler to penetrate the waste
pile. The inner tube is rotated to open and close
the sampler. A thief is used to sample dry granules or powdered wastes, where particle diameter is less than one-third the width of the slots.
Figure 10-2. Thief Sampler
The following procedure is used to collect samples using a thief sampler:
1. While the sampler is in the closed position,
insert it into the sample material from a point
near a top edge or corner, through the center,
and to a point diagonally opposite to the point
of entry.
2. Rotate the inner tube of the sampler into the
open position.
3. Wiggle the sampler a few times to allow
materials to enter the open slots.
4. Place the sampler in the closed position, and
withdraw it from the material being sampled.
5. Place the sampler in a horizontal position with
the slots facing upward.
6. Rotate and slide the outer tube from the inner
tube.
7. Transfer the sample into a laboratory-cleaned
sample container, label the container, and
complete the COC record and the FLB/FN.
8. Clean the sampler on site, or store the contaminated parts of the sampler in a plastic storage tube for subsequent cleaning. Store used
rags in plastic bags for subsequent disposal.

into sticky solids and to loosen soil (see Figure


10-3). A trier samples moist or sticky solids with
a particle diameter less than one-half of its diameter. Triers are available from 61 100 centimeters in length and from 1.27 2.54 centimeters in
diameter. Larger triers can be fabricated.
Figure 10-3. Sampling Trier

The following procedure is used to collect samples using a sampling trier:


1. Insert the trier into the material to be sampled
at a 0- to 45-degree angle from horizontal.
This orientation minimizes spillage of sample.
2. Rotate the trier once or twice to cut a core of
material.
3. Slowly withdraw the trier, making sure that
the slot is facing upward.
4. Transfer the sample into a laboratory-cleaned
sample container using a spatula. Record applicable data in the FLB/FN, and complete the
sample analysis request sheet and COC
record.
5. Clean the sampler on site, or store the contaminated parts of the sampler in a plastic storage tube for subsequent cleaning. Store used
rags in plastic bags for subsequent disposal.
Waste pile samplers are used for sampling wastes
in larger heaps with cross-sectional diameters of
greater than 1 meter (see Figure 10-4). They also
can be used for sampling granular or powdered
wastes, materials in large bins or barges, or soils
where the grain sampler or sampling trier is not
long enough. The waste pile sampler essentially
is a large sampling trier. It is commercially
available or easily fabricated from sheet metal or
plastic pipe. Procedures for using the waste pile
sampler essentially are identical to the sampling
trier.
Figure 10-4. Waste Pile Sampler

A trier consists of a tube cut in half lengthwise


with a sharpened tip that allows the sampler to cut
Chapter 10 Waste Sampling

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10.5.6.4. Characteristics of the Material


Materials to be sampled may be homogeneous or
heterogeneous. Homogeneous material, such as
sand blast abrasive, may not require an extensive
sampling protocol. The DQOs of a sampling
event will determine whether grab or composite
sampling is required. If a positive identification
is made in analyzing a composite sample, then the
discrete samples should be analyzed individually
to determine the true distribution of contaminant
throughout each component of the composite. A
thief or trier sampler (if practical for the particular application) would provide a more representative sample compared with a shovel.
If the waste pile is composed of heterogeneous
material, try to determine the source, nature, and
extent of the deposited waste. If possible, sample
the waste sources contributing to the pile to determine the characteristics of the waste pile. If
any of the waste within a heterogeneous waste
pile is hazardous, the entire waste pile should be
managed as hazardous waste, unless the waste
pile can be separated into hazardous and nonhazardous components.
Waste materials may be affected by their inherent
chemical stability. Weathering and leaching over
time may cause older material to differ in chemical composition from newly deposited material in
the same pile. Heterogeneous material may
undergo chemical reactions resulting in pockets
or layers of different compounds.
Waste piles containing unknown waste can be
sampled using a three-dimensional random sampling strategy. This strategy involves dividing
the pile into a three-dimensional grid system and
numbering each grid section and sampling point
using random-number tables or random-number
generators. This strategy should be used only if
all points within the pile can be accessed.
10.5.6.5. Composite Samples
Compositing a number of individually collected
field samples may help reduce analytical costs.
The disadvantage of sample compositing is a loss
of concentration variance data, whereas the advantage is a more representative sample from the
population that is being sampled. Compositing is
Chapter 10 Waste Sampling

especially useful if the waste pile is homogeneous. Compositing requires that equal amounts of
material from each sample be combined, and
ground, sieved, and/or sufficiently mixed so that
an aliquot sample can be removed for laboratory
analysis. To improve the quality of the composite
sample, follow the compositing considerations
offered in ASTM D6051, Standard Guide for
Composite Sampling and Field Subsampling for
Environmental Waste Management Activities.
If the concentration of a regulated material exceeds regulated levels, the entire waste pile
should be managed as regulated waste, or additional sampling and analyses should be performed
to define regulated and non-regulated material.
To avoid having to resample, field sampling
personnel should collect enough volume to provide for a different compositing scheme or additional individual analyses. This precaution requires initial field samples to be retained until the
laboratory results on the composited sample
become available.
When a waste pile is believed to be heterogeneous, individual random sampling is the preferred
sampling technique.
10.5.7. Containerized Solids
Sampling containerized solid materials (e.g.,
sludge, granulars, and powders) is accomplished
generally with one of the following samplers:

Scoop or trowel
Waste pile sampler
Grain sampler.
Each sample should be taken discretely. Depending on the objective of the sampling event (e.g.,
characterization for disposal), compositing samples in the field or laboratory on a weight/weight
basis prior to analysis may be permissible. The
procedure to collect samples using a waste pile
sampler is discussed in the previous section.
Use the following procedure to collect samples
using a scoop or trowel:
1. Open the container to be sampled.

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2. At specified intervals, take small, equal portions of sample from the surface and immediately below the surface.
3. Transfer the sample into a laboratory-cleaned
sample container, label the container, and
complete the COC record and the FLB/FN.
4. Clean the sampler on site, or store the contaminated sampler in a plastic storage tube for
subsequent cleaning. Store used rags in plastic bags for subsequent disposal.
A grain sampler consists of two slotted telescoping tubes, usually made of brass, stainless steel,
or high-density polyethylene. The outer tube has
a conical, pointed tip on one end that permits the
sampler to penetrate the material being sampled.
The sampler is opened and closed by rotating the
inner tube. Grain samplers are generally 61 100
centimeters long by 1.27 2.54 centimeters in
diameter. The following procedure is used to
collect samples using a grain sampler:
1. Open the container to be sampled.
2. While the sampler is in the closed position,
insert it into granular or powdered material or
waste being sampled from a point near a top
edge or corner, through the center, and to a
point diagonally opposite the point of entry.
3. Rotate the inner tube of the sampler into the
open position.
4. Wiggle the sampler a few times to allow
materials to enter the open slots.
5. Place the sampler in the closed position and
withdraw from the material being sampled.
6. Place the sampler in a horizontal position with
the slots facing upward.
7. Rotate and slide out the outer tube from the
inner tube.
8. Transfer the sample into a laboratory-cleaned
sample container, label the container, and
complete the COC record and the FLB/FN.
9. Clean the sampler on site, or store the contaminated sampler in a plastic storage tube for
subsequent cleaning. Store used rags in plastic bags for subsequent disposal.
Chapter 10 Waste Sampling

10.5.8. Sampling for Lead in Paint


X-ray fluorescence spectrometry and direct laboratory testing may be used to determine the lead
content of paint. However, X-ray fluorescence
spectrometry is generally used only as a screening
test to detect the presence of lead, because certain
interferences can make it unreliable for determining exact concentration. Laboratory testing
should be used to determine the actual concentration of lead in solid materials.
To collect a paint sample suitable for lead determination, use a sharp knife to cut through the
paint. Remove the paint with a clean putty knife,
and place the sample in a clean resealable plastic
bag or appropriate container. Label the plastic
bag or container and record pertinent sample
collection information in the FLB/FN.
A sample of about 2 inches by 2 inches is required for a determination of lead content. Be
sure to take a sample of all layers of paint, because only the lower layer may contain lead.
Avoid including any of the underlying wood,
plaster, metal, or brick in the sample. Wipe the
sampled surface and any paint dust with a wet
cloth or paper towel, and discard the cloth or
towel.
If it is determined that a painted surface is homogeneous throughout the building and the same
paint was applied at the same general time
throughout, the number of samples can be reduced. At a minimum, three or five samples each
from doors, windows, and walls for each floor of
a building should be collected.
The U.S. Department of Housing and Urban
Development recommends that action be taken to
reduce exposure to lead in paint when the lead
content is greater than 0.5% by laboratory testing
or greater than 1.0 mg/cm2 by X-ray fluorescence
spectrometry. When the lead content of a door,
window, or wall sample exceeds the recommended action level, all similar areas should be inspected. Action is especially important when
paint is deteriorating or when infants, children, or
pregnant women are present. Generally, buildings constructed after 1980 are not expected to
contain paint with elevated lead concentrations.
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Lead-contaminated waste generated by public,


commercial, and industrial buildings is subject to
hazardous waste regulations. Analysis of the
waste using the Toxic Characteristic Leaching
Procedure (TCLP) may be required. Leadcontaminated wastes with TCLP levels at or above
5 ppm are defined as hazardous and should be
handled and disposed of in conformance with
hazardous waste laws and regulations.
When lead-based paint is an integral part of
demolition debris, the appropriate way to collect
samples is by coring a representative portion of
the material to be disposed to include both paint
and wood. Because a relatively small amount of
lead is present in the paint film, these wastes may
not fail TCLP, and many can be disposed of as
solid waste. If the waste is lead-based paint chips
or blasting wastes, TCLP should be used on the
waste to determine if it is hazardous. Due to the
more concentrated nature of these wastes, they
will often fail TCLP and require management as a
hazardous waste.
10.5.9. Ashore Oil Spill Sampling
This section discusses methods for collecting
surface ashore samples whenever an oil spill has
occurred from a site or a vessel. A suction device
can be used to collect samples. However, the
statistical design of the sampling program should
be the same no matter what devices are used to
collect samples. Ashore oil spill samples can be
collected by inverting a 4-fluid-ounce jar and
collecting the liquid oil sample and store the
sample at 6C. Tarballs should be collected in
an appropriately sized sample container and
stored at 6C. Shallow pollution samples can
be collected by using one of the following methods.
10.5.9.1. Soil Punch Sampling
A soil punch is a thin-walled tube, 15 20 centimeters long, used to extract short cores from
contaminated locations at beaches. The following
steps are used to collect samples with a soil
punch:
1. Drive the tube into the potentially contaminated location with a wooden mallet.

Chapter 10 Waste Sampling

2. Extract the tube and core.


3. Push the collected materials into a mixing
bowl, place the sample in a labeled container
with a Teflon-lined cap, and store the sample
at 0 6C.
4. Complete the COC record and the FLB/FN.
5. Clean the sampler on site, or store the contaminated parts of the sampler in a plastic storage tube for subsequent cleaning. Store used
rags in plastic bags for subsequent disposal.
10.5.9.2. Scoop or Shovel Sampling
Surface samples following an ashore oil spill are
collected with a scoop and shovel. A small plastic disposable scoop can be used to collect representative samples. Proper QA/QC procedures
should be followed to ensure cross-contamination
cannot occur during sampling events. Larger
representative samples can be collected using a
shovel.
10.5.9.3. Hand Auger Sampling
Shallow surface ashore oil spill samples can be
collected with a hand auger. Samples should not
be used for the examination of a core sample,
because soil is mixed when the auger is pushed
into the ground. The following procedure is used
to collect a sample with a hand auger:
1. Place the hand auger at the location where the
sample is to be collected.
2. Twist or screw the auger, extract the sample,
and pull the auger.
3. Push collected materials into a mixing bowl,
place the sample into a labeled container with
a Teflon-lined cap, and store the sample at
6C.
4. Complete the COC record and the FLB/FN.
5. Clean the sampler on site or store the contaminated parts of the sampler in a plastic storage tube for subsequent cleaning. Store used
rags in plastic bags for subsequent disposal.
Note: Power augers can be used to collect samples. The
procedure is the same as for the hand auger.

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10.6. QA/QC
See Chapter 3 of this handbook for information
on establishing an appropriate QA/QC protocol.
A QA/QC plan involves the establishment of a
sampling protocol, which is designed to minimize
sources of error in each stage of the process, from
sample collection to analysis and reporting of
analytical data. See Chapter 2 for information on
creating a SAP. Key elements of a SAP for waste
sampling are as follows:

Development of a statistically sound sampling


plan for spatial and temporal characterization
of the drums, waste pile, and tanks
Installation of a vertical and horizontal
sampling network to allow for the collection of
subsurface samples
Use of a sampling device that minimizes
disturbance to the chemistry of the media
formation
Use of field decontamination procedures to
minimize cross-contamination during sampling
Collection of QA/QC samples and adherence
to COC procedures.

10.7. Sampling Equipment List


Section 3.8 provides a generic sampling equipment list applicable to most sampling events. The
following list provides additional equipment
applicable to waste sampling. In most cases, only
a portion of the equipment listed below would be
required for a given sampling event.

Manual Drum Opening


- Bung wrench
- Drum deheader
Remote Opening
- Hydraulic device
- Pneumatic device
Ashore Oil Spill Sampling
- 4-ounce jar
Shallow pollution sampling
- Soil punch
- Scoop or shovel
- Hand augers or power auger
Wipe Sampling

Chapter 10 Waste Sampling

- Ruler or measuring tape


- Gauze pad inside a pre-cleaned
container and/or 4-inch diameter
heavy gauge paper, such as Whatman
#4 filter paper
Chip Sampling
- Ruler or measuring tape
- Decontaminated chisel of borosilicate
construction
- Manual or electric hammer
- Natural bristle brush
- Dust pan lined with aluminum foil or
one that is dedicated, decontaminated,
and constructed of a pre-approved
material that will not interfere with the
contaminants of concern
- Aluminum foil
Sweep Sampling
- Natural bristle brush
- Decontaminated stainless steel spatula
and/or a dust pan lined with aluminum
foil, or one that is dedicated,
decontaminated, and constructed of a
pre-approved material that will not
interfere with the contaminants of
concern
- Aluminum foil
Transformer Sampling
- Disposable glass COLIWASA
Containerized Liquids/Drum Sampling
- Bacon bomb, Kemmerer sampler,
weighted bottle sampler, drum thief
(glass tubes), and/or COLIWASA
- Disposable scoop attached to a length
of wooden or plastic rod
Waste Pile Sampling
- Thieves, triers, or shovels
Containerized Solids Sampling
- Scoop or trowel, waste pile sampler,
or grain sampler
Sampling for Lead in Paint
- X-ray fluorescence spectrometer
- Sharp knife to cut through the paint
- Clean putty knife
- Resealable plastic bag or appropriate
container.
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Chapter 10 Waste Sampling

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Chapter 11. Air Sampling


11.1. Purpose
This chapter provides supporting background
information and general procedures for air sampling related to environmental restoration and
compliance issues.
11.2. Scope
Because the requirements and methods for air
sampling are often very complex, this information
is intended only to provide an overview of methods, equipment, and instrumentation. For
specific applications, the established regulatory or
literature reference procedures should be consulted.
11.3. Background
Air sampling is conducted to monitor levels of air
contaminants. Air is the most transient environmental medium and subject to extreme spatial and
temporal heterogeneity. Representative air sampling presents unique and difficult challenges.
Also, the contaminants of interest may be present
at very low concentrations.
11.3.1. Air Matrices
Air sampling matrices include:
Ambient (outdoor) air
Indoor air
Point sources (stacks, exhausts, and other
emission sources)
Fugitive emissions (sources of air pollutants
other than stacks or vents)
Soil gas, particularly over and around landfill
waste sites, or groundwater plumes (soil gas
sampling is addressed in Chapter 4, Soil
Sampling).
In general, ambient or outside air will contain the
smallest concentration of detectable air pollutants, and indoor air will contain an increased
concentration range of pollutants. Pollutant
concentrations from point sources such as stacks
and vents, and fugitive emissions can vary from
ppb levels to almost 100% pollutant.

Chapter 11 Air Sampling

11.3.2. Objectives of Air Sampling and


Monitoring
Air sampling and monitoring may be performed
to:
Determine background levels of contaminants
Provide continuous monitoring of atmospheric or industrial process conditions
Measure acute or periodic releases of contaminants
Provide data for computerized dispersion
modeling to evaluate contaminant patterns
and trends
Vapor intrusion (VI) investigations. See the
DoD Vapor Intrusion Handbook for more information on conducting VI investigations
Monitor and evaluate remediation processes
(e.g., air stripping, soil vapor extraction, and
excavation). See US Army Corps of Engineers EP-200-1-24, Air Pathway Analysis for
the Design of Remedial Action Projects, and
Chapter 11 of this Handbook and for more information.
The basic objective of air monitoring is to representatively measure in situ, or transfer all of the
contaminant from a measured quantity of air into
an analytical instrument that will respond proportionally to the amount of contaminant present. In
practice this includes:
Taking a portable instrument to the contaminated air location
Taking a measured volume of the contaminated air to an instrument in the laboratory or
in the field
Extracting the contaminant from a measured
volume of air and measuring its concentration
in the laboratory or in the field.
Accurate measurements are often difficult to
achieve, because many factors affect air sample
representativeness, quantitation, and minimization of artifacts. Artifacts are contaminants originating from sources other than the intended sample. Common sources of artifacts are:
Contaminated sampling equipment
Improper sampling procedures
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Undesired physical or chemical reactions of


the sample with the sampling container or collection media
Thermal effects
Contamination from adjacent sites or sources
not representative of the site (e.g., indoor
sources during a vapor intrusion investigation)
Emissions from surrounding activities.
In addition, artifacts and poor quantitation are
common problems with air analyses because the
concentrations of contaminants are often very low
with respect to the surface areas of the containers
and sampling media used for their collection.
Many different methods have been developed for
measuring air contamination. The choice of
method for a particular task depends on the anticipated use of the data, required detection/quantitation limits, data turnaround needs,
data quality objectives, and regulatory requirements written into facility operating permits.
11.4. General Classification of Air Pollutants
Generally, air pollutants are broadly classified
into two types gases/vapors and particulates.
Gases such as sulfur dioxide, nitrogen oxides, and
carbon monoxide result primarily from industrial
combustion processes. Hydrogen sulfide and
halogens and their derivatives come mainly from
industrial operations. Solvent vapors have numerous anthropogenic sources and can be present
from primary or secondary sources (vadose zone
and/or ground water contamination).
Hydrocarbons and their oxidation products are
primarily associated with gasoline fuel operations
and incomplete combustion. Ozone results from
photochemical reactions with nitrogen oxides,
hydrocarbons, and other organic compounds.
Particulates can be either droplets of liquid or
solid particles. When particulate matter is suspended in air, it is called an aerosol. Aerosols
most prevalent in pollution are in the 0.01 100
micron diameter particle size range. Aerosols can
be formed by:
Water vapor (e.g., fog or steam)

Chapter 11 Air Sampling

Smoke and industrial fumes


Reaction of species such as sulfur dioxide
with water
Growth of smaller entities such as salts into
agglomerates (e.g., ammonium sulfate and nitrate)
Organic liquid particulates from the distillation or vaporization of volatile materials
Atomization of liquids through a small orifice.
Types of solid particulates include:
Soot or carbon found in smoke from combustion processes of natural or man-made origins
(particles are 0.01 1.0 micron diameter and
very sticky)
Fly ash consisting of non-combustible mineral
solids formed from complete oxidation of
coal or fuel oil, generally <200 micron diameter
Dusts from natural or industrial disintegration
processes, generally 1 1,000 micron diameter
Fumes from condensation, calcination, or
chemical reactions.
Liquid particulates include:
Mists arising from vapor condensation, chemical reactions, or liquid atomization.
Many common types of pollutants are actually
combinations of the general classifications:
Smoke is a combination of gases and solid
and liquid particulates
Solid particulates frequently have organic
and inorganic species adhered to their surfaces
Liquid particulates may combine with
gases and solid particulates
Atmospheric aerosols are frequently mixtures of soluble and insoluble materials,
with relative humidity determining the
equilibrium of the two phases. They may
be chemically complex with volatiles and
several soluble aerosols co-dissolved.
Figure 11-1 illustrates relative particle
size ranges for aerosols, dusts, and fumes.

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Figure 11-1 Particle Size Ranges for Aerosols, Dusts, and Fumes
Source: Faith, W. L. and Atkinson, A. A., Jr

Chapter 11 Air Sampling

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11.5. Factors Affecting Ambient Air Sampling
and Monitoring
11.5.1. Meteorological
11.5.1.1. Meteorological Parameters
Primary meteorological parameters to be considered in ambient air sampling are:
Wind direction
Wind speed
Temperature
Atmospheric stability
Atmospheric pressure
Precipitation.
Wind direction is most critical and must be monitored and documented constantly during air sampling events. Large variations in samples can
result from even momentary shifts in wind direction. Changes in wind speed alter the volatilization rates of liquid contaminants and concentrations of contaminants downwind of the source.
Generally, increased wind speed increases volatilization of liquids at the source and may conversely decrease the concentration of volatile
downwind of the source. Increased wind speed
may have the opposite effect on non-volatiles by
increasing the amounts adsorbed by particulates
such as soil and dust. Increased wind speed
facilitates transfer of a greater number of large
particulates from the source.
Higher temperature also increases volatilization.
Both air temperature and solar radiation are factors, with solar radiation usually most critical,
particularly for compounds with high vapor
pressures.
Atmospheric stability refers to vertical motions of
the air. When atmospheric conditions are unstable, pollutants become more dispersed in the
various vertical layers. Under stable conditions,
downwind concentrations are generally higher.
When monitoring sources such as landfills, atmospheric pressure is a significant factor, affecting the migration of gases through and out of the
source. Low atmospheric pressures favor increased volatilization rates. Precipitation decreases overall airborne contaminants. The highest concentrations of contaminants generally
occur in the initial precipitation samples. This is
Chapter 11 Air Sampling

a result of particulate matter with its precipitate


and gaseous contaminants being physically
scrubbed from the air by the precipitation. Precipitation resulting in 100% relative humidity also
significantly decreases particle transport by wind
and volatilization rates.
11.5.1.2. Meteorological Measurements
For many air dispersion modeling applications,
meteorological parameters can be obtained from
the National Weather Service, the National
Oceanic and Atmospheric Administration
(NOAA), National Climatic Data Center, and the
Federal Aviation Administration (FAA). These
may be hourly observations, or may be readings
taken every 5 15 minutes and calculated to an
hourly average. For certain applications, it may
be necessary to set up a custom on-site
monitoring program. This is important if realtime analysis is needed or if wind flow is
significantly affected by the terrain.
11.5.1.3. Wind Measurements
Wind direction and speed are critical parameters
in predicting contaminant path of travel, air concentration, and deposition rates. Frequently, wind
measurements are made at a height of 10 meters
above ground or equal to the height of the stack
or source being measured. It is very important
that the structure supporting the monitoring
equipment does not in any way interfere with the
wind measurement, nor should any other structure
or topographical factors be close enough to interfere with accurate measurements. The sensors
are generally mounted on a thin mast above the
tower at a height three times the lateral tower
dimension.
Either prop vane or rotating cup anemometers can
be used to measure wind speed. The cup anemometer has the advantage of being independent
of direction, and can be calibrated to within 1%
accuracy. Slowing of wind speed with this type
sensor can lead to 5 10% error if the sensor
continues to rotate. Vane type sensors must be
damped to prevent over rotation, which results in
an artificially high directional variation.

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11.5.1.4. Temperature and Humidity
For the purposes of most modeling, temperature
and humidity measurements that are representative of hourly periods can be used. The sensors
can be located at the height of the shelter or about
1.5 meters. For plumes, temperature is used to
calculate the plume rise from buoyant sources. If
the contaminants of interest are also hygroscopic,
a humidity measurement is also required. Sensors should be protected from direct solar radiation and the buildup of heated air within the
shielded area. This can often be done by aspirating the air flow over the sensors.
Sometimes it is desirable to measure the temperature at two levels, usually between 2 and 10
meters, and use the temperature difference to
determine the degree of atmospheric stability or
surface inversion.
For dry deposition measurements, it is often
necessary to know air humidity, surface wetness,
amount and type of precipitation, and the chemistry of the precipitation.
11.5.2. Topographical Factors
Mountains, hills, valleys, lakes, and seas can
significantly affect wind direction and the dispersion patterns of air pollutants. Wind generally
flows along the axis of valleys with bi-directional
distribution. At night, colder air flows down the
slope into the valley creating thermal inversion of
the air. The result is increased pollutant concentrations in the valley due to decreased vertical air
dispersion. During the daytime hours, the effect
is reversed but to a lesser degree.
Near oceans and large lakes, the differences in
daytime and nighttime temperatures result in bidirectional wind changes. During the day, the
wind generally moves from the cooler body of
water toward the land in an upward motion. At
night as the land mass cools, the effect is reversed
producing "land breezes", which are not as
strong.
11.5.3. Extraneous Contaminant Sources
Extraneous background contamination can come
from many sources. Incidental atmospheric
contaminants such as automobile exhaust or
exhaust from a gasoline powered generator can
Chapter 11 Air Sampling

render samples useless. Incidental contaminants


on the large surfaces of containers and sorbents
used to collect or concentrate samples can also
pose significant problems. Because inadvertent
contamination can affect analytical results, it is
imperative that all sampling equipment be scrupulously clean and many types of blanks run.
11.5.4. Response Time of Sensors
Response time is the time required for a real-time
sensor, recording in situ measurements, to respond to an incremental change in contaminant
concentration and settle to a final value within a
margin of error of the correct contaminant concentration. This is an important criterion to consider when selecting monitoring equipment for a
specific application.
11.5.5. Placement of Samplers and Monitors
Placement requirements for sampling devices and
monitors vary greatly depending on the type of
source, type of monitoring, data quality objectives, and duration of the sampling or monitoring
event. In general, care should be taken to maximize the representativeness of the data and minimize artifacts and effects resulting from poor collector or sensor placement.
When collecting air samples to determine the
effect of an operation or facility on air quality,
there must be at least one upwind sample taken to
determine background ambient air conditions.
The arrangement of downwind samples should
vary depending on site conditions and project
objectives.
Since the movement of airborne contaminants
depends on weather conditions, the weather must
be monitored during sampling. If there is a significant change in wind direction, samplers must
be moved to maintain the proper upwinddownwind arrangement.
Because sampling equipment is often exposed to
the elements, and operates for extended periods
of time, it should be checked frequently to ensure
proper operation. It should also be placed in a
secured area when possible.

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11.6. General Terms
11.6.1. Whole Air versus Component
Samplers
Whole air samples are collected in various types
of plastic bags, glass globes, or metal canisters
with polished inside surfaces. Component samples are collected by passing the air stream
through a filter device, a trapping liquid, or a
solid sorbent medium.
11.6.2. Real Time versus Integrated or
Composite Samplers
Field or "real-time" sampling refers to a variety of
methods, using specific detectors, which can
quickly survey an area of interest. Often these
measurements are used to determine the placement of time integrated samplers, or other samplers for analysis in a laboratory. A grab sample
may also be referred to as a real-time sample
since the duration of collection is usually under a
minute.
Composite or time-integrated samplers collect a
sample or data over a specified time period, either
continuously or periodically and give a representation of air contaminants over a much longer
period of time than a real-time or grab sample.
11.6.3. Active Versus Passive Samplers
Samples may be collected in either an active or
passive mode. Active air samplers use a pump or
vacuum to pull ambient air through the monitor
or collection media. Passive samplers allow
ambient conditions to diffuse the sample through
the monitor or the solid adsorbent material, which
may be covered with a membrane or plastic film.
The samples diffuse through the membrane and
are adsorbed onto the solid media.
11.7. Strategies for Assessment of Air Pollution
Emissions
Several approaches exist for evaluating emission
of air pollutants. The method of choice depends
on the end use of the data, data quality objectives,
availability of sampling equipment, accessibility
of sources, and recommendations of the regulatory agencies. EPA has published a four volume
series for air pathway analysis (APA). These
documents, Air/Superfund National Technical
Chapter 11 Air Sampling

Guidance Study Series, Vols. 1 4 are recommended for details on the various sampling methods. Sampling and Analysis of Airborne Pollutants, edited by Eric D. Winegar and Lawrence H.
Keith, also provides guidance in this area.
11.7.1. Direct Assessment
Generally, it is preferable to measure emission
rates directly rather than determine downwind
mass/volume concentrations, the reason being
that the data has more versatility for use in various modeling applications, where changes in
parameters such as meteorological conditions can
be evaluated. Direct measurements are also more
useful for determining long-term effects, determining National Priority List (NPL) status for
pollutants, and meeting permitting requirements.
They are most useful for volatile contaminants.
The preferred EPA method for these measurements is to set up an isolation flux chamber or
enclosure over a small surface area of the emission site. This method is recommended for:
Land surfaces
Non-aerated, non-mixed liquid surfaces
Aerated, mixed liquid surfaces
Fugitive emissions from processes including
leaks in seams, valves, ports, and controllers.
Advantages include:
Cost effective
Simple equipment requirements
Direct measurements
No models or estimates required
Generally better quality data
No upwind contamination and fewer meteorological interferences.
Disadvantages include:
Not always possible
Primarily used for volatiles materials
Must exercise caution in data extrapolation.
11.7.2. Indirect Assessment
The indirect assessment approach uses a variety
of samples from different ambient locations
relatively close to the source to estimate concentrations via dispersion modeling equations. There
are many models available, some developed for
stack emissions, and others for area sources. The
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plers and weighting of sample data. The models
are designed to determine parameters such as
downwind concentrations (sometimes at different
heights), concentrations directly over the source,
and general area concentrations.
Advantages include:
Can be done where direct measurements are
not feasible or possible
Virtually any volatile or particulate species
can be evaluated
Not dependent on emission measurements
Analyte measurements depend on analysis
technique and sampling media.
Disadvantages include:
Meteorological conditions play a major role
and must be relatively stable for valid data
collection
Possibility of upwind contamination
Lower concentrations of analytes due to
mixing and dispersion forces
Possibility of air flow interferences by topographical features
Can be costly to perform
Complexity of sampling devices
Long term sampling may be difficult due to
changing meteorological and atmospheric
conditions
Labor and analysis intensive
Much more difficult to evaluate specific areas
within a site.
11.7.3. Air Monitoring and Dispersion
Modeling
In this method, measurements are generally made
further downwind of the source and the data are
used in a customized site-specific model to estimate overall site concentrations. For this type of
determination to be accurate, meteorological and
topographical factors must be accurately evaluated in the model. Modeling guidance can be
found in the EPA Superfund Exposure Assessment Manual, Appendix J, which gives a brief
description of EPA and other air pollution models. After a model is chosen, an estimate is made
of source emission and downwind concentrations.
The predicted and actual downwind concentration
data are compared and source concentration is
iteratively varied within the modeling equations
Chapter 11 Air Sampling

until the data fit the equations for source and


downwind concentrations. From the iterative
process, the actual source emission concentration
is thus estimated.
Advantages include:
Can be done at greater distance from the
source
Exact data on source emission not required.
Disadvantages include:
Dispersive forces result in concentrations
being lower further from source
The fit of the model to the actual conditions is
critical
Because the process is iterative, the uncertainty may be large.
11.7.4. Predictive Modeling
This method is based on choosing an emission
model for a specific source type. Data for these
models are usually obtained from literature,
estimated, or calculated. For better accuracy,
some data may need to be determined experimentally. The method is useful when used for screening or when an assessment does not require a high
degree of confidence.
Advantages include:
Fast
Inexpensive
Requires fewer or no field measurement
Useful screening tool.
Disadvantages include:
Provides estimate only
Fit of site source and model critical
Can be very inaccurate.
11.8. Field Measurement Instruments
Instruments have been developed for field operations to allow real-time measurement of air quality. Most instruments are meters, which measure
analyte concentrations by passing a stream of air
through the detector for a finite time interval.
Other instruments monitor continuously and
sound an alarm when a pre-set concentration level
is exceeded, or monitor over a given time period
and determine a time weighted average exposure.
Before using any field instruments, the following
factors must be considered:
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Limitations based on functional design or


manufacturer quality control
Safety must always be considered to ensure
that the chosen instrument is compatible with
the potential hazard. For example, some instruments are capable of detecting explosive
hazards, but not all are safe for operations under these conditions. If the atmospheric concentration is potentially greater than 25% of
the lower explosive limit, the meter itself
must be certified safe for operation. Agencies
certifying equipment safety include Factory
Mutual (FM), Underwriters Laboratory (UL),
and Mine Safety and Health Administration
(MSHA)
Although equipment accuracy may be certified within set limits by the manufacturer or
the National Institute of Occupational Safety
and Health (NIOSH), whenever possible,
equipment should be calibrated before and after use. For some instruments calibration in
the laboratory may be acceptable and will
save time and inconvenience in the field
Operators should be thoroughly familiar with
the instrument and operating instructions before use. Always read or review the manual
prior to using an instrument in the field.
Advantages include:
Immediate readout
Portability.
Disadvantages include:
Response usually is not specific to a single
chemical
Detection limits are generally in the range of
acute health effects (i.e., field instruments
may not have the sensitivity needed to measure low concentrations of pollutants)
Relatively expensive compared with sample
collection equipment
Quality control can be difficult because it is
hard to run blanks and calibration samples in
the field
Changes in temperature and humidity may
affect the sensitivity and accuracy of the instruments.
Field monitoring instruments are widely used for
air monitoring in emergency situations where it is
Chapter 11 Air Sampling

important to know whether the air is safe to


breathe or whether a respirator will have to be
worn. They are also widely used for screening to
determine approximate concentration levels and
the number and placement of other types of samplers. The following sections describe the common types of instruments used to monitor various
air contaminants.
11.8.1. Detection of Volatile Organic
Chemicals (VOCs)
VOCs include components of natural gas, gasoline, and solvents. These chemicals can evaporate to form an explosive mixture in air and may
be toxic at lower concentrations. The following
analytical instruments have been developed as
portable devices, which can be taken into the field
for air monitoring. Each instrument is calibrated
by determining the response of the detector to
clean (unpolluted) air and to air containing a
known concentration of a VOC. When the instrument is used to monitor polluted air, instrument calibration should depend on the type and
concentration of VOCs present.
11.8.1.1. Photo Ionization Detector (PID)
A PID contains a miniature lamp, which emits a
very short wavelength ultraviolet radiation.
Inside the instrument, a small air pump continuously draws ambient air through a tiny chamber, which is flooded with ultraviolet light (See
Figure 11-2). If the radiated energy is higher than
the ionization potential of a particular organic
chemical in the sample, the chemical will be
ionized. The chamber also contains two electrodes charged to a high voltage and attached to a
sensitive current measuring device. When ions
are formed, electric current flows between the
electrodes in proportion to the number of ions in
the air. The instrument display generally has
units of parts-per-million (ppm). This concentration should be interpreted as the equivalent response to the calibration gas, not the ppm of
unknown VOCs in the air, as different chemicals
have different responses to the instrument.
Advantages include:
Stable, calibration remains fairly constant
Easier to ship, no flammable gas is required
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Sensitive to commonly encountered VOCs
Not affected by presence of methane in air.
Disadvantages include:
Sensitive to high humidity
Can have problems when used in below freezing temperatures
Bulb must be cleaned occasionally
Response to various chemicals depends on the
photoionization potential of the chemical and
type of bulb used
Detection limit generally 2 or 3 ppm VOCs
(higher for VOCs not easily ionized by UV
light)
Not specific to a single chemical.
11.8.1.2. Flame Ionization Detector (FID)
A FID works by burning contaminated air in a
hydrogen flame within the instrument. The residue of most burned organic vapors contains
positively charged carbon-containing ions, which
are attracted to the negative collecting electrode
in the chamber. As the ions are collected, a
current is generated, which corresponds to the
concentration of vapor present. The amount of
current is shown on the instrument display.
Advantages include:
Response is more consistent for differing
chemicals than with the PID
Less sensitive to moisture than the PID
Disadvantages include:

Chapter 11 Air Sampling

Figure 11-2 Photo I onization Detector

Need hydrogen for flame


Sensitive to methane, which can mask the
presence of toxic VOCs. Special methane filters are available
Detection limit generally 2 or 3 ppm VOCs in
air
11.8.1.3. Portable Gas Chromatograph (GC)
and Gas Chromatograph/Mass
Spectrometer (GC/MS)
A portable GC adds the benefit of separating
mixtures of chemicals in an air sample. The air to
be analyzed can be collected as either a whole air
sample or in some instruments contaminants can
be adsorbed on collection media and then desorbed to the instrument. Contaminants travel
through a chromatography column and are separated based on their physicochemical properties,
finally reaching a detector that outputs a signal
that is proportional to the concentration of the

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contaminant. Common GC detectors utilize the
same technology as the PID and FID.
A GC/MS utilizes a mass selective detector that
provides structural information on the detected
contaminant (mass spectrum).
Advantages include:
Selectivity, contaminants are separated and
can be identified by both the time they spend
traveling through the chromatography column
and by their mass spectrum
Sensitivity, these instruments are generally
more sensitive than a PID or FID
Disadvantages include:
Powering the instruments may necessitate a
portable generator or large batteries
GC and GC/MS can be more difficult to
operate and require more extensive training
than the handheld instruments.
11.8.1.4. Infrared Radiation Absorbance
Detector
Although VOC vapors are transparent to visible
light, they will absorb infrared radiation. This
detector passes a beam of infrared radiation
through air. The extent to which the different
wavelengths of infrared radiation are absorbed
depends on the chemical present and its concentration. Because different chemicals have different absorbance spectra, the infrared radiation
detector can be used to selectively measure specific chemicals. Some analyzers contain a library
of calibration data for common gases and vapors,
and have the capability to store data for multi
user-calibrated gases.
Advantages include:
Specific for particular chemicals, since different VOCs have different infrared radiation
absorbance characteristics.
Disadvantages include:
Detection limits are generally greater than
those for the PID or FID.
11.8.1.5. Indicator Tubes
Indicator tubes are small glass tubes filled with a
porous material coated with a reagent. When air
is drawn through the tube, the chemical of interest
reacts with the reagent, resulting in a color
change. The length of filler that changes color
Chapter 11 Air Sampling

depends on the concentration of the chemical of


interest. Indicator tubes are available for both
volatile organic and inorganic chemicals such as
ammonia, hydrogen sulfide, sulfur dioxide, nitrogen dioxide, etc. Indicator tubes are available for
use with hand-operated pumps (which draw the
required amount of air through the tube in a
minute or less), battery-operated pumps (which
draw the required amount of air through the tube
over an 8 hour period to provide a measurement
of average air concentration), and diffusion tubes
(which depend on the diffusion of the chemical
into the tube over an 8 hour period).
Advantages include:
Inexpensive
Direct readout.
Disadvantages include:
Sensitivity limited to concentrations of chemicals that cause acute symptoms, hence not
sensitive enough for environmental sampling
where chronic effects are important
Limited accuracy (20 50%)
Not completely selective: Although tubes are
designed to detect single chemicals, other
chemicals present in the air may affect readings
Wet (foggy) weather and low temperatures
can affect reading accuracy
Limited shelf life: Each sampling tube must
be used within a few months to a year of purchase, depending on tube type.
11.8.2. Explosimeter
Explosimeters operate by passing an electric
current through a platinum wire, causing it to heat
up and glow. As air is passed over the hot wire,
any VOCs in the air are oxidized on the surface
of the wire. Oxidation increases the temperature
and electrical resistance of the wire, resulting in a
decrease in the current.
Advantages include:
Rugged
Sensitivity to VOCs is in the percent range,
which is relevant to explosive mixtures.
Disadvantages include:
Does not work if the concentration of oxygen
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clude an oxygen meter to assure that oxygen


is present at proper level
Does not work if hydrogen sulfide (H2S) in
air greatly reduces the meter sensitivity; most
explosimeters also include a H2S meter
Not sensitive to the presence of VOCs at low
levels that may still present toxicity hazards.

11.8.3. Detection of Hydrogen Sulfide (H2S)


H2S is a toxic volatile gas with a permissible
exposure limit of 10 ppm in air. Though hydrogen sulfide has a strong odor of rotten eggs,
exposure to it for more than a few minutes desensitizes the nose, so the odor cannot be used as a
reliable indicator of the presence of hazardous
concentrations. A portable H2S meter has an
electrochemical detector designed specifically to
react to the gas. The meter is calibrated by using
air containing a known concentration of H2S.
11.8.4. Detection of Carbon Monoxide (CO)
CO is a colorless and odorless toxic gas. Portable
CO detectors have an electro-chemical cell,
which reacts specifically to CO. Combination
meters with sensors for explosive gas mixtures,
oxygen, hydrogen sulfide, and CO are available.
Such meters are commonly used to check air
quality in confined spaces prior to entry. CO can
also be measured by non-dispersive infrared
spectroscopy.
11.8.5. Particulates
The Occupational Safety and Health Administration (OSHA) permissible exposure limit (PEL)
for particulates not otherwise regulated (3.5 - 100
m in diameter) is 15 mg/m3. Portable meters are
available that work by passing a stream of air
through a light beam and measuring the amount
of light bouncing off particles present. The resulting measurement indicates the concentration
of particles in the air.
Advantages include:
Real time data
Portable
Disadvantages include:
Sensitive to fog and other aerosols
Not size specific for dust particles
Not easily calibrated in the field
Chapter 11 Air Sampling

11.8.6. Mercury Vapor


Mercury vapor detectors are used primarily to
provide guidance on whether respirators are
needed in areas where mercury has been spilled.
Detectors work by exposing a gold foil to a flow
of contaminated air. Mercury vapor present in
the air is absorbed by the foil, changing its electrical resistance. Approximately 40 ten-second
samples containing 100 g Hg/m3 may be taken
before the sensor reaches saturation. At that
point, a ten-minute heating cycle is manually
activated to clear the accumulated mercury from
the foil.
Advantages include:
Specific to mercury
Portable
Real-time data (response time one to ten
seconds)
Detection limits adequate for work place
monitoring (one to ten g/m3).
Disadvantages include:
Not easily calibrated
Quality control samples such as a blanks and
spikes are difficult in the field
Detects only atomic mercury fumes, not
organic mercury compounds, which are even
more toxic.
11.9. Collecting Samples for Laboratory
Analysis
Air sampling procedures have been developed to
enable representative samples of air or contaminant(s) of interest to be delivered to the laboratory for analysis.
11.9.1. Whole Air Samples
Collection of whole air samples is the simplest
sampling technique. For this method, a sample of
air is collected in a bag, jar, or canister, and the
container is delivered to the laboratory.
A major concern with this type of air sample is
the loss of the chemical of interest due to adsorption on or permeation through the container walls.
Chemical reactions with the container walls and
photochemical reactions induced by sunlight are
also a concern for some compounds. It is important that the holding times be minimized and that
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the samples be analyzed as soon as possible. For
very reactive or low concentration components
this is not a suitable method.
At very high concentrations (e.g., several ppm),
condensation may be a problem. Due to these
limitations, this method should be used only for
very stable volatile and semi-volatile organic
chemicals such as hydrocarbons and chlorinated
hydrocarbons with boiling points less than 150
C.
The following sections describe procedures,
which may be used to collect whole air samples.
11.9.1.1. Bag Samples
Flexible bags for the collection of whole air
samples are available in several different plastic
materials including Tedlar, Teflon, Mylar,
and Saran. Bag sampling is very useful in
emergency situations where light weight and
simplicity are an advantage and where the holding time will be very short.
Advantages include:
Light weight
Easily transportable
Inexpensive.
Disadvantages include:
Short holding times: Leakage and/or permeation of chemicals into and out of the bag can
be a problem. Therefore, flexible bags should
not be used for sampling for very low levels
of air pollutants. Flexible bags are generally
used to collect grab air samples to be analyzed within a few hours
Cleanliness: Even new bags can be a source
of contamination. Their cleanliness should be
verified by blank analysis prior to use. Bags
to be reused must be thoroughly cleaned by
multiple evacuations and fillings with clean
air. Cleanliness of each bag should then be
verified before use. Cleanliness requirements
depend on the concentration of the chemical
to be measured and the analytical method.
Reuse of flexible bags is not recommended
when sampling for very low concentrations of
organics
Complicated field procedures: Additional
equipment is required to fill flexible bags, including a vacuum pump and a hard-sided
Chapter 11 Air Sampling

sampling box. An empty bag is put into the


box and the inlet of the bag is attached to the
sampling port of the box. The valve on the
bag is then opened and the box is sealed. The
vacuum pump is used to pull air out of the
box, which reduces the pressure around the
bag, causing it to fill with ambient air. The
box is then opened and the valve on the bag is
closed. The bag is then removed from the
box, labeled, and delivered to the laboratory
Transparent: Exposure to sunlight may cause
photo-induced reactions of the chemicals in
the air. Must store in darkness (e.g., wrap in
black plastic bags)
Reactivity: Some polymeric bag materials are
reactive with certain compounds.
11.9.1.2. Glass Globe Samplers
Evacuated glass bulbs have been used extensively
to collect whole air samples.
Advantages include:
Ease: Simple to use when collecting grab
samples; just open the valve to let air into the
globe, close the valve, and deliver globe to
the laboratory
Cleanliness: Easily cleaned in the laboratory;
should remain clean in storage
Holding times: Neither absorption nor leakage is a significant problem, so holding
times are longer than with flexible plastic
bags.
Disadvantages include:
Weight: Heavier than plastic bags
Fragile: Subject to breakage in use and transportation
Transparent: Exposure to sunlight may cause
photo-induced reactions of the chemicals in
the air; must store in darkness (e.g., wrap in
black plastic bags)
Reactivity: Surfaces can be reactive to some
compounds.
11.9.1.3. Metal Canister Samplers
Stainless steel canisters, made less reactive by
depositing a pure chrome-nickel oxide on the
interior surface (Summa polishing process),
offer many advantages for collecting whole air
samples. In general, a canister is evacuated to a
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vacuum of approximately 30 inches of Hg. When
opened to ambient air, the differential pressure
causes air to flow into the canister. This technique may be used to collect grab samples (duration of 10 to 30 seconds) or time-integrated samples (duration of 12 to 24 hours) taken through a
flow-restrictive inlet. A mass flow controller can
maintain a constant flow rate from full vacuum to
within about five inches of Hg below ambient
pressure. With a critical orifice flow restrictor, a
decrease in the flow rate occurs as atmospheric
pressure approaches.
Advantages include:
Holding time: Canisters are not subject to
sample permeation or photo-induced chemical
effects. (Sample integrity of trace level organic compounds stored in Summa polished canisters has been demonstrated for many
chemicals for up to 30 days.)
Reusable: Can be reused after cleanup
Cleanliness: Generally, does not absorb
contaminants, so it is relatively easily
cleaned. However, canisters used for high
concentration samples should not be reused
for very low concentration sampling. New
canisters should be checked for cleanliness
before use
Rugged: Not readily breakable
Sampling period: Can be used to collect
either grab samples or samples over a 24 hour
period
Available in larger sizes than glass globes.
Disadvantages include:
Heavy
Expensive.
11.9.2. Air Component Samples
Another method of sampling air is to selectively
remove the chemicals of interest from a measured
volume of air and submit the concentrated sample
to the laboratory for analysis. When obtaining
any sample by selectively removing and concentrating the components of interest from a large
volume of air, it is extremely important to remember that other undesirable things may also be
concentrated such as background artifacts and
water vapor. Because these undesirables may
Chapter 11 Air Sampling

make subsequent analyses difficult or impossible,


every effort should be made at the sampling stage
to eliminate or minimize their inclusion. The
following sections describe some of the sample
concentration methods commonly used. The
following section explains some methods used to
collect and concentrate organic components from
ambient air.
11.9.2.1. Passive Sampling Badges
A passive sampling badge consists of a solid
adsorbent material covered with a membrane or
plastic film. The chemicals of interest diffuse
through the membrane and are adsorbed by the
material inside the badge. The sampling badge is
then put into a non-permeable (foil lined) pouch
or plastic container and sent to a laboratory for
analysis. At the laboratory, the adsorbing material is treated with solvents or heat to release the
absorbed chemicals of interest.
Advantages include:
Simple: no pumps, hoses, or batteries required
Portable: can be attached to a worker's collar
to measure the actual air breathed
Several types of badges are available for
different chemicals:
Volatile organic chemicals
Formaldehyde 0.1 to 5 ppm
Glutaraldehyde 0.2 to 5 ppm
Mercury vapor detection limit < 0.05
mg/m3.
Disadvantages include:
High detection threshold: Suitable for work
place exposure studies where the decision criteria are based on acute health effects. (Not
suitable for most ambient air sampling)
Accuracy: 25%
Requires 8 hour sampling period
Not suitable for sampling for semi-volatile
organic chemicals.
11.9.2.2. Active Air Samplers
These samplers use a pump to pull ambient air
through the collection media. Sampling pumps
are classified as high flow (500 3,000 cm3/min)
or low flow (50 200 cm3/min). Flow rates

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should be maintained within 5% of set rate.
Pump features may include:
Diaphragm or piston-type of pumping action
Flow regulator
Rotameter or strokes counter to measure flow
rate or sample volume
Pulse dampener to smooth flow rate
Timing mechanisms
Safety features for use in flammable or explosive atmospheres.
Various collection techniques are used to sample
the chemicals of interest from the air.
Advantages include:
Chemicals of interest are concentrated, resulting in improved detection limits
Standard methods have been defined and
validated
Samples are collected over long periods to
obtain data on average contaminant levels.
Disadvantages include:
Air flow may change over time need wind
speed and direction data throughout sampling
period
Complex equipment is used, which increases
the likelihood of sampling errors
A source of power may be required for the air
sampling pumps.
11.9.2.3. Solid Sorbents
Solid sorbents are the primary collection means
used to sample volatile and semi-volatile organic
chemical vapors from air. Typically, large volumes of air are passed through a series of cartridges containing an inert adsorbing material.
The organic chemicals are adsorbed from the air
onto the surface of the adsorbent material. The
laboratory extracts the adsorbed chemicals by
using solvents or heat.
Unfortunately, solid sorbents are not selective for
individual chemicals. Since broad classes of
chemicals are adsorbed, the material may become
saturated before the end of the sampling period
and fail to adsorb all of the chemicals of interest
from the air. This potential problem is controlled
by using several sorbent cartridges in series. If
the analysis of the last cartridge does not find any
of the chemical of interest, it was either not
Chapter 11 Air Sampling

present in the air or completely adsorbed by the


material in the preceding cartridges.
A wide variety of solid sorbent materials have
been developed for air sampling.
11.9.2.3.1. Organic Polymers
Tenax. Tenax resin (2,6-diphenylene
oxide polymer) is used in air sampling for volatile organic chemicals with boiling points
between 35 and 100 C (molecular weights
ranging up to several hundred AMU). Use of
Tenax is specified in EPA Method TO-1 and
in stack sampling Method 0030. Tenax must
be specially processed before use to remove
interfering chemicals. The processing procedure is specified in Methods 0030 and 0031.
Amberlite XAD-2. XAD-2, used in air
sampling for polynuclear aromatic hydrocarbons (PAHs), is specified in the following
EPA sampling methods:
Method TO-13
Method 0010 (Modified Method 5
Sampling Train) for stack samples
Method 0020 for stack samples
XAD-2 resin, as supplied by the manufacturer, is impregnated with a bicarbonate salt solution to inhibit microbial growth during storage. Both the salt solution and any residual
extractable monomer and polymer species
must be removed before the resin is used.
Appendix A to EPA Method 0010 gives detailed procedures for preparing XAD-2 sorbent resin.
Thermosorb/N. Thermosorb/N is used to
sample for N-nitrosodimethylamine.
Polyurethane foam. Polyurethane is used to
sample semi-volatile chemicals such as pesticides, PCBs, and dioxins from large volumes
of air, achieving a very low detection limit.
11.9.2.3.2. Inorganic Powders
Includes silica gel, Porasil, Florisil, alumina,
and inorganic molecular sieves. These materials are considerably more polar than organic
polymeric sorbents and thus capture polar compounds. However, the inorganic powders can
become deactivated by adsorbing water moisture
from the air. Silica gel will adsorb compounds
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such as alcohols and phenols and other oxygencontaining compounds such as esters, aldehydes,
and ketones. Florisil can be used to collect
chlorinated pesticides and PCBs from air.
11.9.2.3.3. Carbon Adsorbents
Carbon materials are a much stronger adsorbent
than organic polymers and therefore allow efficient collection of highly volatile organic contaminants such as vinyl chloride, benzene, and
toluene. However, the strong adsorption of carbon adsorbents can be a disadvantage in cases
where recovery by thermal desorption of less
volatile is desired because of the high temperatures required (e.g., 400 C).
There are a variety of carbon based adsorbents
available with widely varying adsorption properties. The commonly available classes of carbon
adsorbents include:
Carbon Molecular Sieves. Sold under trade
names such as Spherocarb, Carbosphere,
Carbosieve, and Ambersorb XE-347,
these materials have been used to sample air
for very volatile organic chemicals such as
vinyl chloride, ethylene dichloride, and methylene chloride.
Carbonaceous polymeric adsorbents are
available under trade names Ambersorb
XE-340, XE-347, and XE-348. XE-340 appears to be useful for volatile compounds in
the C4 to C6 boiling point range, a volatility
range not covered by organic polymeric adsorbents such as Tenax.
Activated carbon. Conventional activated
carbons have a porous structure, which leads
to difficulty in recovering adsorbed materials.
Therefore, this material is rarely used as a
sampling media.
11.9.2.4. Chemical Derivitization Techniques
Ambient air can be exposed to a chemical reagent
that reacts with the volatile organic chemical of
interest, forming a non-volatile product trapped in
the sampling device. Integrated sample collection
and derivitization of carbonyls with 2,4dinitrophenyl hydrazine (DNPH) is a particularly
good example of the utility of concentration and
derivitization methodology.
Chapter 11 Air Sampling

The reagent can be in solution in a liquid impinger or "bubbler" or can be adsorbed on the surface of a porous solid. Liquid impingers require
considerable glassware that must be specially
cleaned, and the liquids must be handled in the
field under difficult conditions. In addition, the
impinger may have to be immersed in a bath of
ice water to prevent the evaporation of the reagent-containing liquid.
Cartridges of solid sorbents coated with derivitizing reagent can provide much higher collection
efficiencies than a liquid impinger. A variety of
sorbent media can be used including: silica gel,
glass beads, glass fiber filters, Amberlite XAD-2
resin, Florisil, Chromosorb P, Carbopak B,
and C18 coated silica. Although the solid phase
method is much superior to the impinger method,
the sampling is not without problems such as:
incomplete collection
reactivity of carbonyls
surface adsorption of carbonyls
artifact and interfering compound formation
blank contamination
variable rates of formation of derivatives for
various compounds
interference of ozone and sulfur dioxide
11.9.2.5. Nebulization/Reflux Concentration
This method is a modification of the bubbler/impinger methodology. In this case, instead
of bubbling air sample through a liquid scrubbing
solution, the liquid is nebulized to a fine mist
inside a glass bulb. Air is introduced through a
small orifice located in close proximity to the
nebulization tip and analytes of interest in the air
flowing through the mist are transferred to the
mist droplets. In the fine mist state, the surface
area for analyte contact is greatly increased,
resulting in significantly improved collection
efficiencies. A non-wettable filter (usually Teflon) collects and coalesces the mist back into the
bulb while passing scrubbed air out. The liquid
scrubber solution can either dissolve the analytes
of interest or chemically derivatize them.
Table 11-1 lists the EPA standard methods for
sampling ambient air and their respective collection media.
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Table 11-1 EPA Standard Air Contaminant Sampling Methods for Toxic Organic
Compounds

Method

Description

TO-1

Tenax GC adsorption and Gas Chromatography/Mass Spectrometry (GC/MS)


analysis

TO-2

Carbon molecular sieve adsorption and


GC/MS analysis

TO-3

Cryogenic trapping and GC/FID or ECD


analysis
High volume PUF sampling and GC/ECD
analysis
Dinitrophenylhydrazine (DNPH) liquid
impinger sampling and HPLC/UV analysis
Aniline liquid impinger with High Performance Liquid Chromatography (HPLC)
Thermosorb/N adsorption
Sodium hydroxide liquid impinger with
High Performance Liquid Chromatography (HPLC)
High volume Polyurethane Foam (PUF)
sampling with High Resolution Gas
Chromatography/High Resolution Mass
Spectrometry (HRGC/HRMS)
Low volume Polyurethane Foam (PUF)
sampling with Gas Chromatography/Electron Capture Detector (GC/ECD)
DNPH coated adsorbent cartridge followed by High Performance Liquid
Chromatography (HPLC) detection
Cryogenic Preconcentration and Direct
Flame Ionization Detection (PDFID)
PUF/XAD-2 adsorption with GC and
HPLC detection
Summa Canister collection with GC Analysis
Summa Canister collection with GC/MS
Analysis

TO-4
TO-5
TO-6
TO-7
TO-8

TO-9

TO-10

TO-11

TO-12
TO-13
TO-14
TO-15

Chapter 11 Air Sampling

Types of Compounds Determined


Volatile, nonpolar organics (e.g., aromatic hydrocarbons, chlorinated hydrocarbons having boiling points in the range
of 80 to 200 C
Highly volatile, nonpolar organics (e.g.,
vinyl chloride, vinylidene chloride,
benzene, toluene) having boiling points
in the range of -15 to +120 C
Volatile, nonpolar organics having boiling points in the range of 10 to 200 C
Organochlorine Pesticides and PCBs
Aldehydes and Ketones
Phosgene
N-Nitrosodimethylamine
Cresol, Phenol

Dioxins (polychlorinated dibenzo-pdioxins), Furans (polychlorinated dibenzofurans)


Pesticides

Formaldehyde

Non-Methane Organic Compounds


(NMOC)
Polynuclear Aromatic Hydrocarbons
(PAHs)
Volatile Organic Compounds
Volatile Organic Compounds

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11.10. Particulates
Many toxic chemicals present in ambient air are
associated with solid particulates or aerosols.
Organic chemicals, such as semi-volatile organics and polar compounds, may adsorb to particulates or condense to varying degrees and exist
in a complex dynamic solid-vapor equilibrium
with particulate matter. Volatile metals, such as
cadmium and lead, in stack gases may condense
on the surface of particulates. Some toxic
compounds such as asbestos are present in
ambient air only as particulates. Air sampling
for particulates uses filtration, centrifugation, or
impaction to remove particles from the air (See
Figure 11-3 for an example of a typical particulate sampler). Certain adsorbed chemicals may
evaporate off the surface of the particles during
the capture process. Therefore, there is often
the need for a gas phase collection device (e.g.,
adsorbent) downstream from the particulate
capturing device. Analysis of both collection
media would be necessary to determine the total
amount of chemical present in the ambient air,
but the results may not describe the actual phase
distribution of the chemical in the air.

Figure 11-3 Particulate Sampler


11.10.1. Fil